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Method for preparing spherical aluminum nitride powder under assistance of high atmospheric pressure and fluoride additive

A fluoride and additive technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., to achieve the effects of large particle size, convenient operation and simple process

Inactive Publication Date: 2014-08-13
天津纳德科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a method for preparing spherical aluminum nitride powder with simple process and low cost in view of the existing problems when aluminum nitride powder is used as a thermally conductive filler

Method used

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  • Method for preparing spherical aluminum nitride powder under assistance of high atmospheric pressure and fluoride additive
  • Method for preparing spherical aluminum nitride powder under assistance of high atmospheric pressure and fluoride additive
  • Method for preparing spherical aluminum nitride powder under assistance of high atmospheric pressure and fluoride additive

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 48.5g of alumina (average particle size 1.1 μm) and 1.5g calcium fluoride into 50 g of deionized water to prepare an aqueous slurry with a solid content of 50 wt%, and add 25 g of carbon black (average particle size of 0.2 μm) into 75 g of water , prepared into aqueous slurries with a solid content of 25%, each ball milled for 24 hours, mixed and then ball milled for 24 hours, then dried and ground. The obtained mixture was placed in a graphite crucible, and transferred to a gas pressure sintering furnace with a nitrogen pressure of 0.9 MPa, and reacted at 1800° C. for 2 h. After the reaction was completed, the obtained product was reacted in a muffle furnace at 650° C. for 4 hours to remove carbon. Use X-ray diffraction to calculate the nitriding rate of the product; use a laser particle size analyzer to measure the average particle size D50 of the product; use an electron scanning electron microscope to observe the product morphology, and randomly select 50 partic...

Embodiment 2

[0031] 48.5g aluminum oxide (average particle diameter 1.1 μm) and 1.5g yttrium oxide are added in 50g deionized water, are mixed with the aqueous slurry that solid content is 50wt%, 25g carbon black (average particle diameter 0.2 μm) is added in 75g water, Aqueous slurries with a solid content of 25% were prepared, and after ball milling for 24 hours, they were mixed and ball milled for 24 hours before being dried and ground. The obtained mixture was placed in a graphite crucible, and transferred to a gas pressure sintering furnace with a nitrogen pressure of 0.9 MPa, and reacted at 1800° C. for 2 h. After the reaction was completed, the obtained product was reacted in a muffle furnace at 650° C. for 4 h to remove carbon. The nitriding rate, average particle size, morphology, sphericity, etc. of the product were characterized by the same method as in Example 1, which are listed in Table 1. Composite materials were prepared by the same method as in Example 1, and the thermal ...

Embodiment 3

[0033]50g of alumina (average particle size 1.1 μm) was added to 50 g of deionized water to prepare an aqueous slurry with a solid content of 50 wt%, and 25 g of carbon black (average particle size of 0.2 μm) was added to 75 g of water to prepare a solid content of 25 wt%. % water-based slurry, after ball milling for 24 hours respectively, after mixing, continue ball milling for 24 hours and then dry and grind. The obtained mixture was placed in a graphite crucible, and transferred to a gas pressure sintering furnace with a nitrogen pressure of 0.1 MPa at normal pressure, and reacted at 1800° C. for 2 h. After the reaction was completed, the obtained product was reacted in a muffle furnace at 650° C. for 4 h to remove carbon. The nitriding rate, average particle size, morphology, sphericity, etc. of the product were characterized by the same method as in Example 1, which are listed in Table 1. Composite materials were prepared by the same method as in Example 1, and the therm...

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Abstract

The invention discloses a method for preparing spherical aluminum nitride powder under the assistance of high atmospheric pressure and a fluoride additive, belonging to the technical field of preparation of non-oxide ceramic powder materials. The method concretely comprises the following steps: evenly mixing aluminum oxide, a carbon source and fluoride additive through a ball-milling technology, drying and then putting in a graphite crucible, transferring into an atmospheric-pressure sintering furnace, performing carbon thermal reduction reaction for 1-6 hours in the nitrogen atmosphere, and maintaining the pressure of nitrogen to be 0.2-2MPa, and the reaction temperature to be 1650-1900DEG C; and after the reaction is completed, putting the obtained product into a muffle furnace, carrying carbon emission for 1-5 hours under the condition of 500-750DEG C, thus obtaining the spherical aluminum nitride powder. The prepared aluminum nitride powder has the characteristics of being high in spherical degree, smooth in the surface, even for particle size distribution and the like, the intermediate particle size is 3-10mu m, and the spherical degree achieves more than 80%; the spherical aluminum nitride powder is very suitable as high-heat-conducting aluminum nitride filler; in addition, the technological method is simple, the raw material cost is relatively low, and large-scale industrial production can be realized.

Description

technical field [0001] The invention relates to a method for directly preparing spherical aluminum nitride powder by carbothermal reduction, in particular to a technology for assisting the preparation of spherical aluminum nitride powder by using high nitrogen pressure and fluoride additives, which belongs to non-oxide ceramic powder The technical field of preparation of bulk materials. Background technique [0002] Aluminum nitride is a covalent compound with a hexagonal wurtzite structure. It has a series of excellent properties such as high theoretical thermal conductivity, low dielectric constant, good insulation, high mechanical strength, and an expansion coefficient that matches silicon chips. , has a wide range of applications in the field of electronic packaging materials, and can be used to prepare high thermal conductivity ceramic substrates and be added to polymers as inorganic fillers to improve the thermal conductivity of composite materials. [0003] At presen...

Claims

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Application Information

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IPC IPC(8): C01B21/072
Inventor 陈克新王琦崔巍葛一瑶
Owner 天津纳德科技有限公司
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