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 nit

Method used

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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

Experimental program
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Example Embodiment

[0062] Example 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 1h to obtain a fluffy white solid substance; after washing the white solid substance with liquid ammonia, vacuum at 120°C (vacuum degree is 5×10 -2 Pa) Dry for 8 hours to obtain silimide;

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

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

Example Embodiment

[0067] Example 2

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

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

[0070] 15wt% of α-Si 3 N 4 Mixed with 75wt% amorphous silicon nitride powder, ball milled at 20°C for 20min, the ball milling speed is 100rpm, the particle size of the amorphous silicon nitride powder after ball milling is 5μm; the...

Example Embodiment

[0072] Example 3

[0073] Pour 500 volumes of toluene and cyclohexane mixed solution with a volume ratio of 300:200 and 200 volumes of liquid ammonia into the reactor at -50°C; 25 volumes of silicon tetrachloride diluted with 125 volumes of toluene, It is added to the reactor through the feeding tube, silicon tetrachloride and liquid ammonia undergo liquid phase interface reaction at -45°C for 1h to obtain a fluffy white solid substance; the white solid substance is washed with liquid ammonia and vacuumed at 120°C (Vacuum degree is 5×10 -2 Pa) Dry for 8 hours to obtain silimide;

[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 3h, and nitrogen flow rate 40mL / min to obtain white fluffy amorphous silicon nitride powder;

[0075] 10wt% of KCl and 90wt% of amorphous silicon nitride powder were ball milled at 20°C for 20 minutes, the ball milling speed was 200 rpm, a...

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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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