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Method for preparing silicon nitride powder through atomization reaction process

A technology of silicon nitride powder and reaction, which is applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of difficult process and storage, difficulty in complete reaction, large surface area of ​​powder, etc., and achieve high α phase content, Effects of no agglomeration and high purity of silicon nitride

Inactive Publication Date: 2015-12-09
SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The technical effect that this new process produces silicone oxide particles having improved properties compared to previous methods can be attributed to their smallness, lower costs, higher purities for silane (SiH 4) molecules, and narrow distributions of sizes.

Problems solved by technology

There have been many technical problem addressed in these inventions relating to making small amounts of highly durable, expensive, strong SiON particles suitable for various applications like electronic components manufacturing. Current techniques involve crushing them into smaller sizes but they still contain contaminants and require complicated steps involving multiple stages.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Control the temperature in the reaction tower to -40°C, add 125L of liquid ammonia, spray silicon tetrachloride into the tower body from the pressure atomizer, the supply rate is 0.3L / min, the total supply is 3L, and the gas used for spraying is High-purity nitrogen, the gas pressure is 3.5MPa.

[0020] After the reaction, the silicon imide solid and the liquid ammonia dissolved in ammonium chloride are discharged, and the silicon imide solid is obtained after filtration. Put the collected powder product into a low-temperature calciner, raise it from room temperature to 500°C in 1 hour, and keep it warm for 8 hours. During this period, ammonia gas is continuously fed in at a rate of 10 L / min, thereby removing the chlorination in the mixed powder. ammonium, finally obtained product 1.45kg.

[0021] Put the purified silicon imide precursor into a tube furnace, raise it from room temperature to 1000°C for 3 hours, and keep it at 1000°C for 3 hours to decompose the precurs...

Embodiment 2

[0023] Control the temperature inside the tower at -37°C, add 125L of liquid ammonia, spray silicon tetrachloride into the tower body from a pressure atomizer, the supply rate is 0.2L / min, the total supply is 3L, and the gas used for spraying is high Pure nitrogen, the gas pressure is 3.5MPa.

[0024] After the reaction, the silicon imide solid and the liquid ammonia dissolved in ammonium chloride are discharged, and the silicon imide solid is obtained after filtration. Put the collected powder product into a low-temperature calciner, raise it from room temperature to 500°C in 1 hour, and keep it warm for 8 hours. During this period, ammonia gas is continuously fed in at a rate of 10 L / min, thereby removing the chlorination in the mixed powder. ammonium, finally obtained product 1.4kg.

[0025] Put the purified precursor into a tube furnace, raise it from room temperature to 1000°C for 3 hours, and keep it at 1000°C for 3 hours to decompose the precursor to produce amorphous ...

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Abstract

The invention discloses a method for preparing a silicon nitride powder through an atomization reaction process. The method comprises the following steps: atomizing tetrachlorosilane through a pressure atomization manner, wherein the atomization gas employs an inert gas; reacting atomized tetrachlorosilane with liquid ammonia at the interface, controlling the temperature in a tower during reaction to -33.5 DEG C or below, and controlling the feed amount of tetrachlorosilane during reaction; keeping warm of a collected powder product at 400-600 DEG C, and removing ammonium chloride in the product; and keeping warm of purified imino silicon at 950-1100 DEG C to decompose imino silicon to generate amorphous silicon nitride, and then keeping warm at 1400-1600 DEG C to perform crystallization processing on amorphous silicon nitride. The method helps to prepare high-quality silicon nitride.

Description

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Claims

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Application Information

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Owner SHANDONG SINOCERA FUNCTIONAL MATERIAL CO LTD
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