Method for preparing micrometer/nanometer spherical silicon nitride powder

A silicon nitride powder, micron-scale technology, applied in chemical instruments and methods, nitrogen compounds, nanotechnology, etc., can solve the uncontrollable content of impurity ammonium chloride, polluted particle shape of silicon nitride powder, by-product ammonium chloride Problems such as clogging can be avoided, and the purity can be easily controlled, the recovery rate is high, and pollution can be avoided.

Active Publication Date: 2016-01-13
陕西阳乐陶瓷材料科技有限公司
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Problems solved by technology

[0013] However, several methods mentioned above to prepare silicon nitride powder have several disadvantages: method (1) is currently the most important industrial production method, but the purity of the product depends on the purity of silicon powder and nitrogen, and in order to improve silicon nitride The silicon nitride powder produced by the powder fineness reaction needs to be broken or ground, and the grinding is easy to cause pollution and cause the particle shape of the silicon nitride powder to be unable to be sph

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  • Method for preparing micrometer/nanometer spherical silicon nitride powder
  • Method for preparing micrometer/nanometer spherical silicon nitride powder

Examples

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Embodiment 1

[0038] Example 1: Place a 500ml quartz glass reactor in a low-temperature bath at -40°C, replace the gas in the reactor with nitrogen for at least 3 times, and fill the reactor with nitrogen. First add 150ml of organic mixed solution and 200ml of liquid ammonia, then add 20g of silicon tetrachloride and stir rapidly with a stirrer.

[0039] The reaction product diimide silicon, ammonium chloride and the remaining unreacted liquid ammonia and organic solution form a yogurt-like loose mixture. After waiting for precipitation for 15 minutes, silicon diimide will be deposited on the lower part of the upper layer 3 liquid ammonia layer of the reaction kettle. The liquid ammonia in the upper layer was extracted, and 100ml of clean liquid ammonia was re-added and stirred. After waiting for 15 minutes for precipitation, the liquid ammonia in the upper layer of the reaction kettle was drawn out, and the ammonium chloride was washed and extracted repeatedly 6 times. When washing and e...

Embodiment 2

[0042] Example 2: Place a 500ml quartz glass reactor in a low-temperature tank at -40°C, replace the gas in the reactor with nitrogen for at least three times, and fill the reactor with nitrogen. First add 150ml of organic mixed solution and 200ml of liquid ammonia, then add 20g of silicon tetrachloride and stir rapidly with a stirrer.

[0043] The reaction product diimide silicon, ammonium chloride and the remaining unreacted liquid ammonia and organic solution form a creamy loose mixture. After waiting for precipitation for 30 minutes, diimide silicon will be deposited in the lower part of the upper layer 3 liquid ammonia layer of the reaction kettle. The liquid ammonia in the upper layer was extracted, and 100ml of clean liquid ammonia was re-added and stirred. After 30 minutes of precipitation, the liquid ammonia in the upper layer of the reaction kettle was drawn out, and the ammonium chloride was washed and extracted repeatedly 8 times. When washing and extracting, the...

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Abstract

The invention discloses a method for preparing micrometer/nanometer spherical silicon nitride powder. The method comprises that liquid silicon tetrachloride is added into liquefied ammonia and an organic solution in a quartz glass reactor, the mixture undergoes a reaction to obtain a yoghourt-type mixture, after deposition, liquid ammonia in an upper layer is drawn, clean liquid ammonia is added into the mixture, the mixture is stirred and precipitated, impurity ammonium chloride is extracted, the reactor and silicam are transferred into a heating furnace, the organic solution is stirred and dried and then is heated to produce amorphous silicon nitride powder, and the amorphous silicon nitride powder is transferred into a silicon carbide or silicon nitride container and then is roasted to form crystalline silicon nitride powder. Silicam powder is prepared by a low temperature reaction, is washed and extracted by liquid ammonia, is purified by ammonium chloride and is subjected to multitime heat treatment to form high-purity micrometer/nanometer spherical silicon nitride powder. The method has a fast preparation rate, a high yield and a high recovery rate, easily controls and improves silicon nitride powder purity and realizes industrial large-scale production.

Description

technical field [0001] The present invention relates to a preparation method of high-purity micron nano-scale silicon nitride powder, in particular to the preparation of diimide silicon by reacting high-purity silicon tetrachloride in high-purity liquid ammonia and organic solution, and the preparation of diimide silicon Purification and heat treatment to prepare high-purity micron nanoscale spherical silicon nitride powder. Background technique [0002] As an important member of the family of high-temperature structural ceramics, silicon nitride ceramics have excellent mechanical properties, thermal properties and chemical stability, such as high room temperature strength and high temperature strength, high hardness, corrosion resistance, oxidation resistance and Good thermal shock resistance and mechanical shock performance, so it is considered by the material science community to be an excellent comprehensive performance, the most application potential and the most promis...

Claims

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Application Information

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IPC IPC(8): C01B21/068B82Y30/00
Inventor 杨乐袁济青
Owner 陕西阳乐陶瓷材料科技有限公司
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