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Method for preparing equiaxed alpha-phase silicon nitride powder

A technology of phase silicon nitride powder and phase silicon nitride, which is applied in the field of inorganic non-metallic materials, can solve the problems of difficult densification of ceramic products, reduce the mechanical properties and thermal properties of silicon nitride ceramics, etc. Shape and size, the effect of easy control of shape

Active Publication Date: 2019-04-12
浙江英德赛半导体材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, the nucleated silicon nitride is easy to preferentially grow into a one-dimensional structure such as nanowires or nanobelts along a certain direction. When silicon nitride with this shape is used as a ceramic sintering raw material, the ceramic product is difficult to be dense. Reduce the mechanical and thermal properties of silicon nitride ceramics

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  • Method for preparing equiaxed alpha-phase silicon nitride powder
  • Method for preparing equiaxed alpha-phase silicon nitride powder
  • Method for preparing equiaxed alpha-phase silicon nitride powder

Examples

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Embodiment 1

[0063] Pour 500 volumes of diluent xylene and 200 volumes of liquid ammonia into the reaction kettle at -60°C; add 25 volumes of silicon tetrachloride diluted with 125 volumes of toluene into the reaction kettle through the feeding tube, four Silicon chloride and liquid ammonia react at the liquid phase interface at -50°C for 1 hour to obtain a fluffy white solid substance; after washing the white solid substance with liquid ammonia, vacuum it at 120°C (vacuum degree is 5×10 -2 Pa) drying for 8 hours to obtain silicon imine;

[0064] Pour the dried white solid silicon imide into a graphite crucible, place it in a tube furnace, and thermally decompose it under the conditions of 900°C, heat preservation for 2h, and nitrogen flow rate of 40mL / min to obtain white fluffy amorphous silicon nitride powder ;

[0065] 15wt% α-Si 3 N 4 Mix with 75wt% amorphous silicon nitride powder, ball mill for 20min at 20°C, the ball milling speed is 100rpm, the particle size of the amorphous sil...

Embodiment 2

[0068] Pour 500 volumes of toluene and 200 volumes of liquid ammonia into the reaction kettle at -20°C; add 25 volumes of silicon tetrachloride diluted with 125 volumes of toluene into the reaction kettle through the feeding tube, silicon tetrachloride React with liquid ammonia at -50°C for 0.5h at the liquid phase interface to obtain a fluffy white solid substance; after washing the white solid substance with liquid ammonia, vacuum it at 120°C (vacuum degree is 5×10 -2 Pa) drying for 8 hours to obtain silicon imine;

[0069] Pour the dried white solid into a graphite crucible, place it in a tube furnace, and thermally decompose it under the conditions of 1000°C, heat preservation for 1h, and ammonia flow rate of 60mL / min to obtain white fluffy amorphous silicon nitride powder;

[0070] 15wt% α-Si 3 N 4 Mix with 75wt% amorphous silicon nitride powder, ball mill for 20min at 20°C, the ball milling speed is 100rpm, the particle size of the amorphous silicon nitride powder afte...

Embodiment 3

[0073] Pour 500 volumes of a mixed solution of toluene and cyclohexane with a volume ratio of 300:200 and 200 volumes of liquid ammonia into a reaction kettle at -50°C; 25 volumes of silicon tetrachloride diluted with 125 volumes of toluene, Add it into the reaction kettle through the feeding tube, and react silicon tetrachloride and liquid ammonia at the liquid phase interface at -45°C for 1 hour to obtain a fluffy white solid substance; after washing the white solid substance with liquid ammonia, vacuum it at 120°C (vacuum degree is 5×10 -2 Pa) drying for 8 hours to obtain silicon imine;

[0074] Pour the dried white solid into a boron nitride crucible, place it in a tube furnace, and thermally decompose it under the conditions of 1000°C, heat preservation for 3h, and nitrogen flow rate of 40mL / min to obtain white fluffy amorphous silicon nitride powder;

[0075] 10wt% KCl and 90wt% amorphous silicon nitride powder were ball-milled at 20°C for 20 minutes, the milling speed ...

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Abstract

The invention discloses a method for preparing equiaxed alpha-phase silicon nitride powder. The method comprises the steps that with silicon tetrachloride and liquid ammonia as raw materials, a silicon imine solid is synthesized under a liquid phase condition, and then the silicon imine solid is thermally decomposed to obtain amorphous silicon nitride; the amorphous silicon nitride and auxiliary additives are treated by a ball milling process for full and uniform mixing; the obtained mixture is put into a graphite or boron nitride crucible, crystallization is carried out for 0-48 hours in an atmosphere sintering furnace under a certain atmosphere condition, and then the equiaxed high-alpha-phase silicon nitride powder with few impurities is obtained. The preparation process of the siliconnitride powder is short in period, the particle morphology of silicon nitride is easy to control, and large-scale industrial production is facilitated.

Description

technical field [0001] The invention relates to a method for preparing equiaxed α-phase silicon nitride powder, which belongs to the field of inorganic non-metallic materials. Background technique [0002] Silicon nitride ceramics have the characteristics of high temperature resistance, good chemical stability, high mechanical strength, and self-lubrication. They are widely used in cutting ball bearings and other wear-resistant parts, high-temperature ceramic bearings, and high-temperature resistant parts for automobile engines. Compared with aluminum nitride ceramics and alumina ceramics, high thermal conductivity silicon nitride ceramics have both high thermal conductivity and high mechanical strength. In addition, during the demoulding process of polysilicon, the α-phase silicon nitride powder does not react with molten silicon, which is suitable for the requirements of crucible coating in the process of purifying polysilicon. High-quality silicon nitride raw material po...

Claims

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Application Information

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IPC IPC(8): C04B35/584C04B35/626C01B21/068
CPCC01B21/068C01P2002/72C01P2004/03C01P2004/62C01P2006/80C04B35/591C04B35/626
Inventor 谢志鹏胡尊兰
Owner 浙江英德赛半导体材料股份有限公司
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