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Micron-sized spherical silicon nitride and preparation method thereof

A silicon nitride, micron-scale technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve problems such as high requirements for equipment and sites, difficult industrial production, poor particle sphericity, etc., to meet production needs. , The particle size is uniform and controllable, and the sphericity is good.

Inactive Publication Date: 2020-06-09
ANHUI ESTONE MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The spray granulation method requires the use of a spray dryer, which has high requirements for equipment and sites; the high-pressure carbothermal reduction method needs to be reacted in a high-temperature and high-pressure environment, which is dangerous and difficult for industrial production, and the sphericity of the prepared particles is poor

Method used

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  • Micron-sized spherical silicon nitride and preparation method thereof
  • Micron-sized spherical silicon nitride and preparation method thereof
  • Micron-sized spherical silicon nitride and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Mix deionized water, methanol, and concentrated ammonia water according to the volume ratio of 9:9:2, place in a water bath and heat to 40°C and keep the temperature constant, and obtain solution A evenly by magnetic stirring, according to the ratio of 3:2 Weigh phenyltrimethoxysilane and tetraethyl silicate, stir them evenly in a beaker to obtain solution B, add solution B to solution A, stir at a speed of 600r / min for 10min, then stop stirring, stand still After 2 hours, the final solution was collected by centrifugation at a speed of 10000rpm, and dried in an oven at 100°C for 24 hours. The SEM image of the obtained silica spheres is as follows: figure 1 shown.

[0035] (2) Place the silicon dioxide powder obtained in step 1 in an alumina crucible, put it into a tube furnace, then carry out two vacuum pumping treatments, and then feed high-purity nitrogen gas. The nitrogen flow rate is set to 300mL / min, and the heating rate is Set at 5°C / min, keep warm at 1475°C...

Embodiment 2

[0041] (1) Mix deionized water, ethanol, and concentrated ammonia water according to the volume ratio of 9:9:2, place in a water bath and heat to 25°C and keep the temperature constant, and obtain solution A evenly by magnetic stirring, according to the ratio of 3:2 Weigh phenyltrimethoxysilane and tetraethyl silicate, stir them evenly in a beaker to obtain solution B, add solution B to solution A, stir at a speed of 600r / min for 10min, then stop stirring, stand still After leaving for 2 hours, the final solution was collected by centrifugation at a rotational speed of 10000 rpm, and dried in an oven at 100° C. for 24 hours to obtain the intermediate silica microspheres.

[0042] (2) Place the silicon dioxide powder obtained in step 1 in an alumina crucible, put it into a tube furnace, then carry out two vacuum pumping treatments, and then feed high-purity nitrogen gas. The nitrogen flow rate is set to 300mL / min, and the heating rate is Set at 5°C / min, keep warm at 1450°C for ...

Embodiment 3

[0045] (1) Mix deionized water, methanol, and concentrated ammonia water according to the volume ratio of 3:15:2, place in a water bath and heat to 40°C and keep the temperature constant, and obtain solution A evenly by magnetic stirring, according to the ratio of 3:2 Weigh phenyltrimethoxysilane and tetraethyl silicate, stir them evenly in a beaker to obtain solution B, add solution B to solution A, stir at a speed of 600r / min for 30min, then stop stirring, stand still After leaving for 2 hours, the final solution was collected by centrifugation at a rotational speed of 10000 rpm, and dried in an oven at 100° C. for 24 hours to obtain the intermediate silica microspheres.

[0046] (2) Place the silicon dioxide powder obtained in step 1 in an alumina crucible, put it into a tube furnace, then carry out two vacuum pumping treatments, and then feed high-purity nitrogen gas. The nitrogen flow rate is set to 300mL / min, and the heating rate is Set at 5°C / min, keep warm at 1475°C fo...

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Abstract

The invention discloses a preparation method of micron-sized spherical silicon nitride, belonging to the technical field of inorganic nonmetal powder materials. According to the invention, an improvedStober method is adopted for preparing silicon dioxide containing a benzene ring; and the particle size of the silicon dioxide is controlled by adjusting a water-alcohol ratio, reaction time and reaction temperature, so the particle size of silicon nitride is controlled and is allowed to be uniform and controllable. The prepared spherical silicon nitride can completely maintain the spherical morphology of silicon dioxide, and has good sphericity degree, high purity and an alpha-Si3N4 content of greater than 99%; and the Stober method and a carbothermal reduction nitridation method used in preparation process are mature industrial production methods, technological process is simple, and production requirements can be met.

Description

Technical field: [0001] The invention relates to the technical field of inorganic non-metallic powder materials, in particular to a micron-sized spherical silicon nitride and a preparation method thereof. Background technique: [0002] Silicon nitride ceramics have excellent high temperature resistance, wear resistance, corrosion resistance, good mechanical properties and chemical stability, and are widely used in the machinery industry, chemical industry, aerospace and atomic energy industries. Due to the relatively complex structure of silicon nitride, it was believed that its thermal conductivity was very low in the early stages. In 1995, Haggerty et al. proposed that the complex crystal structure is not the reason for the low thermal conductivity of silicon nitride, but is caused by lattice defects and impurities. [0003] Compared with the widely used alumina (38-42W / m K) thermal conductive filler, silicon nitride has a higher thermal conductivity of ~155W / m K, and sil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/068B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B21/0685C01P2002/72C01P2004/03C01P2004/32C01P2004/50C01P2004/52C01P2004/61C01P2004/64C01P2006/80
Inventor 王伟蒋学鑫王韶晖郭敬新
Owner ANHUI ESTONE MATERIAL TECH CO LTD
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