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Method for directly preparing high-sphericity silicon nitride powder by high pressure and additives

A silicon nitride powder, high sphericity technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of insufficient filling degree and low thermal conductivity, and achieve low production cost, smooth surface, reduced interface effect

Active Publication Date: 2018-06-19
天津纳德科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the problems of insufficient filling degree and low thermal conductivity when the silicon nitride powder material is used as a thermally conductive filler, the present invention provides a method of directly preparing high-sphericity silicon nitride powder with simple process and low cost by using high air pressure and additives The method of solid body overcomes the shortcomings of the prior art. The average particle size of the obtained spherical powder is between 3 and 10 μm, the distribution is uniform, and the sphericity is above 0.8, which greatly improves the filling degree and thermal conductivity of silicon nitride thermally conductive fillers. Conductivity

Method used

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  • Method for directly preparing high-sphericity silicon nitride powder by high pressure and additives
  • Method for directly preparing high-sphericity silicon nitride powder by high pressure and additives
  • Method for directly preparing high-sphericity silicon nitride powder by high pressure and additives

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 7.05g of silicon oxide and 1g of potassium oxide were added to 40g of deionized water to form an aqueous slurry with a solid content of 15wt%, and 7.05g of graphite was added to 40g of deionized water to form an aqueous slurry with a solid content of 15wt%. After ball milling for 2 hours, continue ball milling for 2 hours after mixing, then dry and grind; place the obtained mixture in a graphite crucible, and transfer it to an air pressure sintering furnace, and react for 8 hours at a nitrogen pressure of 0.2 MPa and 1200 °C; after the reaction is completed, you will get The product was reacted in a muffle furnace at 750°C for 1 h to remove carbon.

[0035] product testing

[0036] (1) Use an X-ray diffractometer to analyze the composition of the product, use a laser particle size analyzer to measure the average particle size D50 of the product, use a scanning electron microscope to observe the product morphology, and randomly select 50 particles from the product to mea...

Embodiment 2

[0040]10g of silicon oxide and 2g of calcium fluoride were added to 40g of deionized water to form an aqueous slurry with a solid content of 20wt%, and 10g of carbon black was added to 40g of deionized water to form an aqueous slurry with a solid content of 20wt%. After ball milling for 24 hours, continue ball milling for 24 hours after mixing and dry grinding; place the obtained mixture in a graphite crucible, and transfer it to an air pressure sintering furnace, and react for 8 hours at a nitrogen pressure of 0.3MPa and 1400°C; after the reaction is completed, you will get The product was reacted in a muffle furnace at 650°C for 4h to remove carbon.

[0041] The product detection method is the same as in Example 1.

Embodiment 3

[0043] 10g of silicon oxide and 2g of calcium fluoride were added to 40g of deionized water to form an aqueous slurry with a solid content of 20wt%, and 10g of carbon black was added to 40g of deionized water to form an aqueous slurry with a solid content of 20wt%. After ball milling for 24 hours, continue ball milling for 24 hours after mixing, then dry and grind; place the obtained mixture in a graphite crucible, and transfer it to an air pressure sintering furnace, and react for 3 hours at a nitrogen pressure of 3Mpa and 1800°C; after the reaction is completed, the obtained The product was reacted in a muffle furnace at 650°C for 4 hours to remove carbon.

[0044] The product detection method is the same as in Example 1.

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Abstract

The invention belongs to the field of inorganic nonmetallic powder materials, relates to methods for directly preparing spheric silicon nitride powder through carbothermic reduction and particularly relates to a method for directly preparing high-sphericity silicon nitride powder by adopting high atmospheric pressure and additives. The method is characterized by comprising the following steps of treating silica, carbon powder and the additives by a ball milling process so as to carrying out uniform mixing thoroughly, putting the obtained mixture into a graphite crucible, carrying out a carbothermic reduction reaction in a furnace, putting the carbothermic reduction product into a muffle furnace, and carrying out heat preservation for 1 to 5 hours at the temperature of 600 DEG C to 750 DEG C so as to remove superfluous carbon, thereby obtaining the silicon nitride powder with high sphericity, good dispersity and high phase purity. When the silicon nitride powder is used as heat conducting filler, a final heat-conducting composite product is high in solid-phase filler level and high in heat conductivity, so that the application potential is relatively good. The spheric silicon nitride powder is simple in preparation process and relatively low in raw material cost, so that the implementation of large-scale industrial production is facilitated.

Description

technical field [0001] The invention relates to a method for directly preparing spherical silicon nitride powder by carbothermal reduction, in particular to a method for preparing high-sphericity silicon nitride powder in one step with the assistance of high nitrogen pressure and additives, which belongs to inorganic non-metallic powder materials field. Background technique [0002] The emergence of integrated circuits marks a major progress in the miniaturization and low energy consumption of electronic components. It is not only closely related to our lives, but also widely used in computers, mobile phones and televisions. It also promotes the development of communications, transportation and aerospace industries. develop. With the miniaturization of integrated circuits and the increase of operating frequency, heat dissipation has become a major problem restricting the development of integrated circuits. [0003] Polymeric materials can be used as thermal interface mater...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/068
Inventor 陈克新孙思源王琦葛一瑶
Owner 天津纳德科技有限公司
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