A kind of preparation method of self-catalyzed high-purity aluminum nitride

An aluminum nitride, autocatalytic technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of poor fluidity, long reaction time, high cost, and ensure stability and consistency, diffusion and penetration rate. The effect of increasing and bonding ability

Active Publication Date: 2022-03-01
SHANDONG HENGJING NEW MATERIAL CO LTD
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] Among the various methods of manufacturing aluminum nitride, aluminum powder direct nitriding method, carbothermal reduction method, chemical vapor deposition method, self-propagating combustion synthesis method and microwave synthesis method all have high cost, mass production and synthetic nitriding Aluminum crystal form has defects, low purity and other disadvantages, and the prepared aluminum nitride powder has complex morphology, which leads to poor fluidity and it is difficult to achieve a high filling density, which affects the thermal conductivity of the material
Although the traditional carbothermal reduction method can realize large-scale production, the synthesis temperature is high, the reaction time is long, and the purity of the obtained aluminum nitride is low.

Method used

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  • A kind of preparation method of self-catalyzed high-purity aluminum nitride
  • A kind of preparation method of self-catalyzed high-purity aluminum nitride
  • A kind of preparation method of self-catalyzed high-purity aluminum nitride

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Embodiment 1

[0048] Embodiment 1: The preparation method of self-catalyzed high-purity aluminum nitride in this embodiment is as follows:

[0049] (1) Mixture:

[0050] (1.1) Feeding: Use a clean towel to wipe off the dust and foreign matter on the surface of the aluminum hydroxide powder, carbon powder, aluminum nitride powder raw material bag, add 72 kg of aluminum hydroxide powder, 39 kg of carbon powder, and 2.0 kg of aluminum nitride powder to mix In the mixing tank on the machine, tighten the screw on the mixing tank to fix the lid, start the mixer, control the speed at 15 rpm, and mix for 12 hours to obtain the mixed material;

[0051] (1.2) Unloading: After mixing according to the specified time, control the switch of the mixer so that the outlet of the mixer is vertically downward, wipe off the dust on the outer surface of the mixing tank and the outlet with a clean towel, and put the pre-prepared The good raw material barrel is placed under the discharge port, and the valve is o...

Embodiment 2

[0062] Embodiment 2: the difference between this embodiment and embodiment 1 is:

[0063] The weight of aluminum hydroxide powder is 70 kg, the weight of carbon powder is 36 kg, and the weight of aluminum nitride powder is 2.2 kg;

[0064] During mixing, the rotating speed of the mixer was 12 revs / min, and the mixing time was 18 hours;

[0065] In the reaction furnace, the flow rate of the mixed gas flow is controlled at 0.4L / min, the pressure of the mixed gas flow is controlled at 0.2MPa, the feed rate of propane accounts for 1.0% of the nitrogen, the temperature in the reaction furnace is 1350°C, and the crucible is placed on the push plate Automatically advance a board every 12 minutes;

[0066] The decarburization temperature in the oxidation furnace is 600°C, and the time is 2 hours;

[0067] Other operations are the same.

Embodiment 3

[0068] Embodiment 3: the difference between this embodiment and embodiment 1 is:

[0069] The weight of aluminum hydroxide powder is 60 kg, the weight of carbon powder is 30 kg, and the weight of aluminum nitride powder is 1.6 kg;

[0070] During mixing, the rotating speed of the mixer was 20 rpm, and the mixing was done for 12 hours;

[0071] In the reaction furnace, the flow rate of the mixed gas flow is controlled at 0.5L / min, the pressure of the mixed gas flow is controlled at 0.3MPa, the feed rate of propane accounts for 1.2% of the nitrogen, the temperature in the reaction furnace is 1400°C, and the crucible is placed on the push plate Automatically advance a board every 14 minutes;

[0072] The decarburization temperature in the oxidation furnace is 700°C, and the time is 1.7 hours;

[0073] Other operations are the same.

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Abstract

The invention discloses a method for preparing self-catalyzed high-purity aluminum nitride, which belongs to the technical field of aluminum nitride synthesis, and comprises the following steps: (1) mixing materials: aluminum hydroxide powder, carbon powder, and aluminum nitride powder are used as the The raw materials are uniformly mixed according to a certain weight ratio to obtain a mixed material; (2) high-temperature synthesis: the mixed material is placed in a mixed gas flow of nitrogen and propane at a certain pressure at 1350-1420 ° C, and reacted for 1.5-3 hours to obtain a reaction product ; (3) Decarburization: remove the carbon in the reaction product to obtain aluminum nitride powder. In the preparation method of self-catalyzed high-purity aluminum nitride disclosed by the present invention, aluminum nitride is selected as a seed crystal, and the reaction is carried out in a mixed gas flow of nitrogen and propane at a certain pressure, the thermal motion of reaction molecules is enhanced, and the diffusion and penetration rate is increased. It has a self-catalytic effect, shortens the reaction synthesis time, and reduces the reaction synthesis temperature by 200-400°C; and avoids the pollution of impurity elements brought in by adding other additives, and ensures the purity of the prepared aluminum nitride.

Description

technical field [0001] The invention relates to a method for preparing self-catalyzed high-purity aluminum nitride, which belongs to the technical field of aluminum nitride synthesis. Background technique [0002] Aluminum nitride has excellent characteristics such as high thermal conductivity, low dielectric constant, good insulation, high mechanical strength, and expansion coefficient matching that of silicon chips. It is an excellent circuit substrate and white LED red phosphor (CaAlSiN3:Eu) One of the raw materials, the market demand is large, and the application prospect is broad. [0003] For aluminum nitride ceramic materials, the properties of aluminum nitride, such as morphology, purity, particle size, oxygen content and other impurities, directly affect the thermal conductivity and other properties of aluminum nitride ceramic materials and subsequent sintering and molding processes. For example, when the impurity content in the aluminum nitride powder is too high,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/072C04B35/581C04B35/626
CPCC01B21/0726C04B35/581C04B35/62605C04B35/6265C04B35/62675C04B35/6268C01P2006/80C04B2235/3218C04B2235/422
Inventor 田玉伟许永宾许士铭
Owner SHANDONG HENGJING NEW MATERIAL CO LTD
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