Preparation method of aluminum nitride powder

Abstract

The invention relates to a method for preparing aluminum nitride powder. The method for preparing the aluminum nitride powder comprises the following steps that pseudo-boehmite gel, an inorganic carbon source, a water-soluble organic carbon source and a sintering agent are mixed, and a mixture is obtained; in a nitrogen atmosphere, the mixture is nitrogenized at the temperature of 1,250 DEG C to 1,700 DEG C, and a reduction product is obtained; under the aerobic condition, the reduction product is calcined for 3-10 hours at the temperature of 600 DEG C to 720 DEG C, and the aluminum nitride powder is obtained. The aluminum nitride powder prepared through the method is high in purity.

Description

technical field

[0001] The invention relates to the field of ceramic materials, in particular to a method for preparing aluminum nitride powder. Background technique

[0002] Aluminum nitride ceramic materials have high thermal conductivity, excellent electrical properties, relatively excellent mechanical properties, and a thermal expansion coefficient that matches silicon, as well as excellent oxidation resistance and thermal shock resistance. They are high power density integrated circuits, high power Ideal heat dissipation packaging material for LED and IGBT modules.

[0003] The current preparation methods of aluminum nitride powder mainly include: carbothermal reduction method, aluminum powder nitriding method, high temperature self-propagating method, sol-gel method, gas phase method, etc., wherein, carbothermal reduction method and aluminum powder nitriding method are There are currently two methods suitable for mass production.

[0004] The carbothermal reduction m...

Examples

preparation example Construction

[0025] like figure 1 Shown, the preparation method of the aluminum nitride powder of one embodiment, comprises the following steps:

[0026] Step S110: Mix pseudo-boehmite gel, inorganic carbon source, water-soluble organic carbon source and sintering aid to obtain a mixture.

[0027] Wherein, the mass percent content of the pseudo-boehmite gel is 5-30%. Pseudo-boehmite gel can be purchased from the market or prepared. like figure 2 Shown, the preparation method of pseudo-boehmite gel is as follows:

[0028] Step S210: reacting aluminum hydroxide and sodium hydroxide in water to obtain an aqueous solution of sodium metaaluminate.

[0029] The steps of reacting aluminum hydroxide and sodium hydroxide in water are as follows: according to the volume mass ratio of 10 milliliters: 2 grams to 6 grams, adding aluminum hydroxide to an aqueous solution of sodium hydroxide with a concentration of 10 to 40% by mass , Stir the reaction at 90-110°C to obtain an aqueous solution of s...

Embodiment 1

[0049] The preparation process of the aluminum nitride powder of the present embodiment is as follows:

[0050](1) Preparation of pseudoboehmite gel: according to the volume to mass ratio of 10 milliliters: 4 grams, aluminum hydroxide is added to an aqueous solution of 25% sodium hydroxide by mass percentage, and stirred at 100 ° C React to obtain an aqueous solution of sodium metaaluminate; at 40°C, pass carbon dioxide into the aqueous solution of sodium metaaluminate for 50 minutes, neutralize to a pH value of 11, and then dropwise add mass at a rate of 1 drop in 3 minutes The percentage concentration is 5% ammonia water, continue to pass into carbon dioxide until the pH value is 9, obtain the pseudo-boehmite gel that the mass percentage content of pseudo-boehmite is 25%, wherein, the feeding flow rate of carbon dioxide is 8Nm 3 / h.

[0051] (2) Mix pseudo-boehmite gel, inorganic carbon source, water-soluble organic carbon source and sintering aid by ball milling to make p...

Embodiment 2

[0057] The preparation process of the aluminum nitride powder of the present embodiment is as follows:

[0058] (1) Preparation of pseudo-boehmite gel: according to the volume to mass ratio of 10 milliliters: 2 grams, adding aluminum hydroxide to a 10% aqueous sodium hydroxide solution by mass percentage, stirring and reacting at 90°C, Obtain an aqueous solution of sodium metaaluminate; under the condition of 25°C, pass carbon dioxide into the aqueous solution of sodium metaaluminate for 120 minutes, neutralize until the pH value is 10, and then add the mass percent dropwise at a rate of 1 drop in 5 minutes Concentration is 5% ammonia water, continues to feed carbon dioxide until the pH value is 8.5, obtains the pseudo-boehmite gel that the mass percentage content of pseudo-boehmite is 5%, wherein, the feeding flow rate of carbon dioxide is 2Nm 3 / h.

[0059] (2) Ball milling and mixing pseudo-boehmite gel, inorganic carbon source, water-soluble organic carbon source and sint...

technical field

[0001] The invention relates to the field of ceramic materials, in particular to a method for preparing aluminum nitride powder. Background technique

[0002] Aluminum nitride ceramic materials have high thermal conductivity, excellent electrical properties, relatively excellent mechanical properties, and a thermal expansion coefficient that matches silicon, as well as excellent oxidation resistance and thermal shock resistance. They are high power density integrated circuits, high power Ideal heat dissipation packaging material for LED and IGBT modules.

[0003] The current preparation methods of aluminum nitride powder mainly include: carbothermal reduction method, aluminum powder nitriding method, high temperature self-propagating method, sol-gel method, gas phase method, etc., wherein, carbothermal reduction method and aluminum powder nitriding method are There are currently two methods suitable for mass production.

[0004] The carbothermal reduction m...

Examples

preparation example Construction

[0025] like figure 1 Shown, the preparation method of the aluminum nitride powder of one embodiment, comprises the following steps:

[0026] Step S110: Mix pseudo-boehmite gel, inorganic carbon source, water-soluble organic carbon source and sintering aid to obtain a mixture.

[0027] Wherein, the mass percent content of the pseudo-boehmite gel is 5-30%. Pseudo-boehmite gel can be purchased from the market or prepared. like figure 2 Shown, the preparation method of pseudo-boehmite gel is as follows:

[0028] Step S210: reacting aluminum hydroxide and sodium hydroxide in water to obtain an aqueous solution of sodium metaaluminate.

[0029] The steps of reacting aluminum hydroxide and sodium hydroxide in water are as follows: according to the volume mass ratio of 10 milliliters: 2 grams to 6 grams, adding aluminum hydroxide to an aqueous solution of sodium hydroxide with a concentration of 10 to 40% by mass , Stir the reaction at 90-110°C to obtain an aqueous solution of s...

Embodiment 1

[0049] The preparation process of the aluminum nitride powder of the present embodiment is as follows:

[0050](1) Preparation of pseudoboehmite gel: according to the volume to mass ratio of 10 milliliters: 4 grams, aluminum hydroxide is added to an aqueous solution of 25% sodium hydroxide by mass percentage, and stirred at 100 ° C React to obtain an aqueous solution of sodium metaaluminate; at 40°C, pass carbon dioxide into the aqueous solution of sodium metaaluminate for 50 minutes, neutralize to a pH value of 11, and then dropwise add mass at a rate of 1 drop in 3 minutes The percentage concentration is 5% ammonia water, continue to pass into carbon dioxide until the pH value is 9, obtain the pseudo-boehmite gel that the mass percentage content of pseudo-boehmite is 25%, wherein, the feeding flow rate of carbon dioxide is 8Nm 3 / h.

[0051] (2) Mix pseudo-boehmite gel, inorganic carbon source, water-soluble organic carbon source and sintering aid by ball milling to make p...

Embodiment 2

[0057] The preparation process of the aluminum nitride powder of the present embodiment is as follows:

[0058] (1) Preparation of pseudo-boehmite gel: according to the volume to mass ratio of 10 milliliters: 2 grams, adding aluminum hydroxide to a 10% aqueous sodium hydroxide solution by mass percentage, stirring and reacting at 90°C, Obtain an aqueous solution of sodium metaaluminate; under the condition of 25°C, pass carbon dioxide into the aqueous solution of sodium metaaluminate for 120 minutes, neutralize until the pH value is 10, and then add the mass percent dropwise at a rate of 1 drop in 5 minutes Concentration is 5% ammonia water, continues to feed carbon dioxide until the pH value is 8.5, obtains the pseudo-boehmite gel that the mass percentage content of pseudo-boehmite is 5%, wherein, the feeding flow rate of carbon dioxide is 2Nm 3 / h.

[0059] (2) Ball milling and mixing pseudo-boehmite gel, inorganic carbon source, water-soluble organic carbon source and sint...

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