Preparation method for low-oxygen spherical aluminum nitride powder

A low oxygen content, aluminum nitride technology, applied in the field of high-temperature liquid-phase assisted trimming of aluminum nitride powder morphology, can solve the problems of increasing the contact area of ​​inorganic/organic materials, reducing material performance, and difficulty in achieving high performance

Active Publication Date: 2009-09-09
TSINGHUA UNIV
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  • Abstract
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Problems solved by technology

However, the target use of aluminum nitride obtained by these methods is to prepare aluminum nitride ceramic blocks or substrates by sintering as raw materials, so the particle size of the obtained aluminum nitride powder is ultrafine, generally around 1 μm, and the The particle size of the product reaches 0.5 μm, which will increase the contact area of ​​inorganic/organic materials when used as a thermally conductive filler in organic-inorganic composite materials, increase a large amount of contact thermal resistance, and make it difficult to form an efficient fast channel during heat transfer (thermal conduction chain), and it is difficult to achieve the desired high performance. Therefore, in organic/inorganic high thermal conductivity composite materials, it is desirable that the particle size of the thermally conductive filler be as large as possible to reduce the interface and thereby reduce the resulting thermal resistance.
At the same time, the aluminum nitride powder obtained by these synthesis methods has a relatively uniform appearance except for the relatively uniform appearance obtained by the gas p

Method used

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  • Preparation method for low-oxygen spherical aluminum nitride powder
  • Preparation method for low-oxygen spherical aluminum nitride powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Aluminum nitride accounting for 60% of the total weight (self-propagating synthetic aluminum nitride powder, nitrogen content 32.12wt%, oxygen content 2.02wt%, average particle size 1.2um); accounting for 40% of the total weight of spheroidized oxygen removal After the auxiliary material (calcium carbonate, analytically pure) is mixed (ball milled for 24 hours), it is packed into a graphite crucible with a certain density (calculated in terms of porosity, loose packing, and the porosity is about 45%). 2 Heated to 1800 degrees Celsius in the atmosphere and kept for 3 hours. After the product was crushed and decarbonated, the test results showed that the average particle size of the obtained aluminum nitride particles was 6.8um, the nitrogen content was 33.72wt%, and the oxygen content was 0.25wt. %, the carbon content is 0.09%. The sphericity is 95%. The XRD collection of collections (before and after pickling) of the product obtained in the present embodiment is shown ...

Embodiment 2

[0026] Aluminum nitride (self-propagating synthetic aluminum nitride powder, nitrogen content 32.12wt%, oxygen content 2.02wt%, average particle size 1.2um) accounting for 50% of the total weight; spheroidized oxygen removal accounting for 50% of the total weight The auxiliary material (which is 80wt% calcium carbonate + 20wt% boron oxide mixed, analytically pure) is mixed (ball milled for 24 hours) and packed into graphite with a certain density (calculated by porosity, loose packing, porosity about 45%) inside the crucible, at N 2 Heated to 1750 degrees Celsius in the atmosphere and kept for 3 hours. After the product was crushed and decarbonated, the test results showed that the average particle size of the obtained aluminum nitride particles was 5.2um, the nitrogen content was 33.52wt%, and the oxygen content was 0.35wt. %, the carbon content is 0.10%. The sphericity is 97%.

Embodiment 3

[0028] Aluminum nitride (self-propagating synthetic aluminum nitride powder, nitrogen content 32.12wt%, oxygen content 2.02wt%, average particle size 1.2um) accounting for 80% of the total weight; spheroidized oxygen removal accounting for 20% of the total weight The auxiliary material (which is 70wt% calcium carbonate + 30wt% boron oxide mixed, analytically pure) is mixed (ball milled for 24 hours) and packed into graphite with a certain density (calculated by porosity, loose packing, porosity about 45%) inside the crucible, at N 2 Heated to 1600 degrees Celsius in the atmosphere and kept for 16 hours. After the product was crushed and decarbonated, the test results showed that the average particle size of the obtained aluminum nitride particles was 7.2um, the nitrogen content was 33.42wt%, and the oxygen content was 0.38wt. %, the carbon content is 0.13%. The sphericity is 91%.

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Abstract

The invention provides a preparation method for low-oxygen spherical aluminum nitride powder and pertains to the field of non-oxide ceramic powder material preparation technology. The low-oxygen spherical aluminum nitride powder can be obtained through the following steps: ball-grinding, evenly mixing and then drying aluminum nitride powder and appropriate amount of spherical auxiliary materials for deoxidation; placing the mixture in a graphite crucible with certain loading density, heating to 1,550 to 1,900 DEG C in N2 or Ar and preserving for 0 to 20 hours, and then cooling with the crucible; mechanically crashing the product and heating to 600 DEG C in a muffle furnace for carbon emission, then washing in a hydrochloric acid solution with 5 to 20 mass percent concentration and fully washing the product after acid cleaning in de-ionized water for 2 to 10 times; after drying, obtaining the aluminum nitride powder with 3 to 15mum median particle diameter, more than 90 percent sphericity and less than 1wt percent oxygen content. The preparation method provided by the invention can achieve spherical particle morphology and granulation at the same time required by the high thermal-conductivity aluminum nitride filling.

Description

technical field [0001] The invention discloses a method for preparing spherical aluminum nitride powder with low oxygen content, and relates to a method for assisting in trimming the morphology of aluminum nitride powder in a high-temperature liquid phase. The invention belongs to the technical field of preparation of non-oxide ceramic powder materials. Background technique [0002] Aluminum nitride is an important inorganic non-metallic ceramic material. It has high theoretical thermal conductivity, high insulation, high mechanical strength, and also has excellent anti-oxidation and thermal shock properties. Therefore, AlN is considered as a promising ceramic material. The most important application of aluminum nitride ceramic materials is concentrated in the field of high thermal conductivity electronic packaging materials, including high thermal conductivity aluminum nitride ceramic substrates and adding high thermal conductivity inorganic fillers to polymer matrix comp...

Claims

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Application Information

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IPC IPC(8): C04B35/581C04B35/626
Inventor 陈克新任克刚
Owner TSINGHUA UNIV
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