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Method for producing A1Npowder with microwave carbon thermoreduction cooling-down catalysis calcination

A low-temperature catalysis and microwave technology, applied in chemical instruments and methods, inorganic chemistry, nitrogen compounds, etc., can solve the problems of high cost, long time, high synthesis temperature, etc., and achieve the effect of simple operation, simple equipment and low synthesis temperature

Inactive Publication Date: 2009-05-13
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The raw material cost of this process is higher, the synthesis temperature is higher, and the time is longer

Method used

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  • Method for producing A1Npowder with microwave carbon thermoreduction cooling-down catalysis calcination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] First, mix 100g of industrial aluminum hydroxide with 3g of ammonium chloride, add 50ml of deionized water, and perform wet ball milling for 30min at a ball milling speed of 300r / min. After ball milling, wash with boiling while stirring, the boiling time is 30min, filter with suction, then wash with boiling for three times as above, filter with suction, dry to obtain the mixture of treated ammonium chloride and aluminum hydroxide. Then take 100g of the treated mixture of ammonium chloride and aluminum hydroxide and mix it with 77g of acetylene black, add 3.5g of aluminum powder, and ball mill with absolute ethanol for 5 hours at a speed of 300r / min. Dry after ball milling to obtain a precursor powder with fine particle size and uniform mixture of carbon and aluminum. Then put the precursor into a microwave high-temperature sintering furnace, set the temperature regime, and raise the temperature to 1200°C at a rate of 15°C / min in an ordinary nitrogen atmosphere, and keep...

Embodiment 2

[0038]First, mix 100g of industrial aluminum hydroxide with 9g of ammonium chloride, add 50ml of deionized water, and perform wet ball milling for 30min at a ball milling speed of 300r / min. After ball milling, wash with boiling while stirring, the boiling time is 30min, the stirring speed is 300r / min, and suction filtration. Boil and wash three times as above, filter with suction, and dry to obtain a mixture of treated ammonium chloride and aluminum hydroxide. Then take 100g of the treated mixture of ammonium chloride and aluminum hydroxide and 28g of acetylene black, add 15g of aluminum powder, and use absolute ethanol as the medium for ball milling for 5 hours at a speed of 300r / min. Dry after ball milling to obtain a precursor powder with fine particle size and uniform mixture of carbon and aluminum. Then put the precursor into a microwave high-temperature sintering furnace, set the temperature regime, and raise the temperature to 1350°C at a rate of 25°C / min under an ordi...

Embodiment 3

[0040] First, mix 100g of industrial aluminum hydroxide with 15g of ammonium chloride, add 50ml of deionized water, and perform wet ball milling for 30min at a ball milling speed of 300r / min. After ball milling, wash with boiling while stirring, the boiling time is 30min, the stirring speed is 300r / min, and suction filtration. Boil and wash five times as above, filter with suction, and dry to obtain a mixture of treated ammonium chloride and aluminum hydroxide. Then take 100g of the treated mixture of ammonium chloride and aluminum hydroxide and mix it with 23g of acetylene black, add 25g of aluminum powder, and ball mill it with absolute ethanol for 5 hours at a speed of 300r / min. Dry after ball milling to obtain a precursor powder with fine particle size and uniform mixture of carbon and aluminum. Then put the precursor into a microwave high-temperature sintering furnace, set the temperature regime, and raise the temperature to 1300°C at a rate of 35°C / min in an ordinary ni...

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Abstract

A method for preparing AlN powder by catalytic calcination, temperature reduction to a low temperature, and microwave carbon thermal reduction comprises the following steps: (1), aluminum hydroxide and ammonium chloride are mixed, wetly milled, filtered and dried, so as to obtain a mixture of the ammonium chloride and the aluminum hydroxide; (2), the product obtained in step (1) and acetylene black are mixed, aluminum powder is added to the mixture, and the wet milling and the drying are performed, so as to obtain precursor powder with uniform mixed carbon and aluminum; (3), the precursor obtained in step (2) is put into a high-temperature sintering furnace, and the nitrogen is introduced into the furnace, so as to carry out a microwave carbon thermal reduction-nitridation reaction; and (4), the product obtained in step (3) is calcined in dry air, so as to prepare the aluminum powder. The invention has the advantages of simple process, low synthesis temperature, low material cost, simple equipment, short process flow, simple operation, high purity of the product and environmental friendliness. Furthermore, the invention is suitable for the fields of precision ceramics, electrons, aviation / aerospace and the like, can realize mass industrial production, and has good market prospect.

Description

technical field [0001] The invention relates to a method for preparing aluminum nitride powder by catalytic calcination at lower temperature, in particular to a method for preparing AlN powder by microwave carbothermal reduction with lower temperature catalytic calcination. Background technique [0002] AlN is a covalent compound with a hexagonal wurtzite structure and a density of 3.26 g / cm 3 , The decomposition temperature is 2480°C under normal pressure. As a high-performance ceramic, aluminum nitride ceramics have a series of excellent properties such as high thermal conductivity, high mechanical strength, low thermal expansion coefficient, low dielectric constant and dielectric loss, non-toxic, and insulation, so they are regarded as A new generation of ideal semiconductor heat dissipation substrates and packaging materials for electronic devices is widely used in the electronics industry and is increasingly valued. [0003] To obtain AlN ceramics with excellent prope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/072
Inventor 肖劲陈燕彬周峰
Owner CENT SOUTH UNIV
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