Method for compounding high-quality low-oxygen low-iron aluminium nitride powder

A synthesis method and technology of aluminum nitride, applied in nitrogen compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of short reaction time and high cost, and achieve the effects of short reaction time, low cost and simple equipment

Inactive Publication Date: 2016-03-16
烟台同立高科新材料股份有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

This method also has disadvantages: firstly, excess C must be de-Cized in dry air at 600-900°C after the reaction is complete; There is a relationship between type and performance, different types of raw materials, the difference in nitriding temperature can reach more than 200°C
[0019] The characteristics of this method are: the reaction time is short, AlN powder with good sintering activity can be obtained, and the purity is high, but it is limited by equipment and expensive

Method used

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  • Method for compounding high-quality low-oxygen low-iron aluminium nitride powder
  • Method for compounding high-quality low-oxygen low-iron aluminium nitride powder

Examples

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Effect test

Embodiment 1

[0037] Use aluminum powder with a particle size of D50 of 10 μm and a purity greater than 99.9% as raw material, mix 2000g of aluminum powder with 5000g of aluminum nitride and 240g of ammonium chloride evenly, and sprinkle it on aluminum nitride with a length of 1 meter, a width of 0.2 meters, and a groove depth of 0.2 meters. In the ceramic sagger, then evenly sprinkle 20g of carbon powder with a purity greater than 99.9% on the surface of the mixed powder, place the aluminum nitride ceramic sagger in a high-pressure industrial reactor, and then vacuumize the high-pressure industrial reactor to 1 ×10-4MPa, after the vacuuming is completed, let the pretreated nitrogen gas (the pretreated nitrogen gas refers to the nitrogen gas whose purity is greater than 99.999% to remove oxygen, carbon dioxide, carbon monoxide and water vapor), the pressure is 5MPa, keep for 5min, ignite, Carry out self-propagating high-temperature synthesis, the synthesis temperature is greater than 2000°C,...

Embodiment 2

[0039] Use aluminum powder with a particle size of D50 of 10 μm and a purity greater than 99.9% as raw material, mix 2000g of aluminum powder with 5000g of aluminum nitride and 240g of ammonium chloride evenly, and sprinkle it on aluminum nitride with a length of 1 meter, a width of 0.2 meters, and a groove depth of 0.2 meters. In the ceramic sagger, the aluminum nitride ceramic sagger was placed in a high-pressure industrial reactor, and then the high-pressure industrial reactor was vacuumed to 1×10-4MPa, and after the vacuuming was completed, the pretreated nitrogen gas (pre- The treated nitrogen refers to nitrogen with a purity greater than 99.999% except oxygen, carbon dioxide, carbon monoxide and water vapor), the pressure is 5 MPa, kept for 5 minutes, ignited, and self-propagating high-temperature synthesis is carried out. The synthesis temperature is greater than 2000 ° C and the synthesis time is 10 to 12 minutes. , After the resulting composition is cooled to 20°C by a...

Embodiment 3

[0041] Use aluminum powder with a particle size of D50 of 10 μm and a purity greater than 99.9% as raw material, mix 2000g of aluminum powder with 5000g of aluminum nitride and 240g of ammonium chloride evenly, and sprinkle it on aluminum nitride with a length of 1 meter, a width of 0.2 meters, and a groove depth of 0.2 meters. In the ceramic sagger, the aluminum nitride ceramic sagger was placed in a high-pressure industrial reactor, and then the high-pressure industrial reactor was vacuumed to 1×10-4MPa, and after the vacuuming was completed, the pretreated nitrogen gas (pre- The treated nitrogen refers to nitrogen with a purity greater than 99.999% except oxygen, carbon dioxide, carbon monoxide and water vapor), the pressure is 5.5 MPa, kept for 5 minutes, ignited, and self-propagating high-temperature synthesis is carried out. The synthesis temperature is greater than 2000 ° C and the synthesis time is 10 ~ After 12 minutes, the obtained composite was cooled to 20°C by a wa...

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Abstract

The invention relates to a method for compounding high-quality low-oxygen low-iron aluminium nitride powder, which comprises steps: aluminite powder, aluminium nitride and ammonium salt are uniformly mixed to obtain a mixture according to quality radio of (5-10): (10-40), the mixture is uniformly spread into an aluminium nitride ceramic saggar, then carbon power is uniformly spread on the surface layer of the mixture, the quality radio of the aluminite powder and the carbon powder is 60:1-180:1, a reactor is vacuumized to 1*10-4MPa through a vacuum pump, the aluminium nitride ceramic saggar which is filled with materials is put into a reactor cavity, nitrogen which is pretreated is pumped into the aluminium nitride ceramic saggar for 15-30 min in 5-8MPa, and fully diffuses to contact with the aluminite powder, is compounded in a self-propagating mode by being ignited to obtain a reactant, and the reactant is the high-quality low-oxygen low-iron aluminium nitride powder after being cooled. The method for compounding high-quality low-oxygen low-iron aluminium nitride powder breaks down reaction barriers to fully diffuse by adding the carbon power, vacuumizing the reactor in advance, treating nitrogen, pumping the nitrogen into the reactor in advance and keeping the nitrogen in high pressure for 15-30min, and is low in energy consumption, high in efficiency and obvious in oxygen removal effect.

Description

technical field [0001] The invention relates to a synthesis method of high-quality, low-oxygen and low-iron aluminum nitride powder, belonging to the field of chemical synthesis. Background technique [0002] Aluminum nitride ceramics have excellent properties such as high thermal conductivity, high bending strength, low dielectric constant, and low thermal expansion coefficient. It is a promising functional and structural material that can be used in the field of electronic packaging, and at the same time Suitable for high temperature and corrosive environments. The submicron-sized aluminum nitride powder can be used as an ideal material on the electronic package substrate when the Fe content is less than 35ppm and the O content is less than 1.2wt%. [0003] High-quality aluminum nitride powder is the key factor in determining these applications. It is difficult to synthesize aluminum nitride powder with high purity, low cost, low oxygen content, low iron content and stabl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/072
Inventor 郭大为吕东陈成
Owner 烟台同立高科新材料股份有限公司
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