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Method for preparing high-purity silicon nitride powder by ammonolysis method

A technology of silicon nitride powder and silicon nitride, which is applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of slow production efficiency of silicon nitride, and achieve the effect of easy control and improved production efficiency

Active Publication Date: 2021-07-23
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a method for preparing high-purity silicon nitride powder by ammonium solution, which solves the problem of slow production efficiency of existing silicon nitride

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  • Method for preparing high-purity silicon nitride powder by ammonolysis method

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Embodiment 1

[0030] like figure 1 As shown, the embodiment of the present invention provides a method for preparing high-purity silicon nitride powder by ammonia ammonia solution, comprising the following steps:

[0031] 1. Preparation of silicon nitride precursor

[0032] 1.1. Add solvent and silicon tetrachloride to the reaction vessel. The types of solvents are dichloroethane and hexane. Both dichloroethane and hexane are insoluble in water, that is, ensure that the solvent is dry and avoid silicon tetrachloride from being damp. The reaction occurs, which affects the preparation of high-purity silicon nitride, and the molar mass ratio of the two is arbitrary. The molar ratio between the solvent and silicon tetrachloride is 0:1, and the temperature in the container is controlled at -25°C. The pressure is the value at which the ammonia gas just starts to liquefy at the current temperature. After decompression, the liquid ammonia can be vaporized. At the same time, the liquid ammonia, sol...

Embodiment 2

[0041] like figure 1 As shown, the embodiment of the present invention provides a method for preparing high-purity silicon nitride powder by ammonia ammonia solution, comprising the following steps:

[0042] 1. Preparation of silicon nitride precursor

[0043] 1.1. Add solvent and silicon tetrachloride to the reaction vessel. The types of solvents are dichloroethane and hexane. Both dichloroethane and hexane are insoluble in water, that is, ensure that the solvent is dry and avoid silicon tetrachloride from being damp. The reaction will affect the preparation of high-purity silicon nitride, and the molar mass ratio of the two is arbitrary. The molar ratio between the solvent and silicon tetrachloride is 4:1, and the temperature in the control container is -25~-35°C , the pressure in the container is the value at which the ammonia gas has just started to liquefy at the current temperature. After decompression, the liquid ammonia can be vaporized, and at the same time, the liqu...

Embodiment 3

[0051] like figure 1 As shown, the embodiment of the present invention provides a method for preparing high-purity silicon nitride powder by ammonia ammonia solution, comprising the following steps:

[0052] 1. Preparation of silicon nitride precursor

[0053] 1.1. Add solvent and silicon tetrachloride to the reaction vessel. The types of solvents are dichloroethane and hexane. Both dichloroethane and hexane are insoluble in water, that is, ensure that the solvent is dry and avoid silicon tetrachloride from being damp. The reaction occurs, which affects the preparation of high-purity silicon nitride, and the molar mass ratio of the two is arbitrary. The molar ratio between the solvent and silicon tetrachloride is 1:1, and the temperature in the container is controlled at -30°C. The pressure is the value at which the ammonia gas just starts to liquefy at the current temperature. After decompression, the liquid ammonia can be vaporized. At the same time, the liquid ammonia, sol...

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Abstract

The invention provides a method for preparing high-purity silicon nitride powder by an ammonolysis method, and relates to the field of silicon nitride preparation. The method for preparing the high-purity silicon nitride powder by the ammonolysis method comprises the following steps: adding a solvent and silicon tetrachloride into a reaction container, controlling the temperature and pressure in the container, fusing liquid ammonia into the solvent, and reducing the pressure in the container, so that the liquid ammonia is gasified and boiled so that the whole reaction system is disturbed, and a silicon nitride precursor is obtained; and burning, crushing and roasting the silicon precursor to obtain the silicon nitride. The reactants are in full contact, the generation efficiency of the silicon nitride precursor is high, the particle size of the silicon nitride precursor can be controlled through the solvent amount and the liquid ammonia introduction gasification speed, and control over the particle size of the final product silicon nitride is facilitated.

Description

technical field [0001] The invention relates to the technical field of household kitchens, in particular to a method for preparing high-purity silicon nitride powder by an ammonolysis method. Background technique [0002] Silicon nitride is an important structural ceramic material. It has high hardness, lubricity, and wear resistance. It is an atomic crystal; it resists oxidation at high temperatures. Its physical properties are not much different from those of titanium nitride. Titanium nitride has excellent physical and chemical properties, such as high strength, high hardness, high temperature resistance, wear resistance, and acid and alkali corrosion resistance. Silicon nitride is often used to manufacture mechanical components such as bearings, steam turbine blades, mechanical seal rings, and permanent molds. Similarly, silicon nitride also has a production process similar to that of titanium nitride. [0003] When the applicant applied for the present invention, aft...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/068
CPCC01B21/068C01P2006/80
Inventor 许立信刘岳韩召万超
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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