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A method for preparing Aln nano-powder by plasma-assisted high-energy ball milling

A technology of high-energy ball milling and plasma, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of large dislocation defects, high grain internal energy, high conversion rate, etc., and meet the requirements of reducing high temperature resistance and reducing Composite temperature, energy saving effect

Inactive Publication Date: 2016-06-01
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems existing in the existing combustion synthesis method, the present invention proposes a method for preparing AlN nano-powder by means of mechanical force activation and The method for synthesizing ultra-fine aluminum nitride powder by carbothermal reduction combined with dielectric barrier discharge plasma activation is characterized by simple operation, low cost, smaller grain size, larger dislocation defects, and smaller grain size than aluminum nitride prepared by ball milling alone. High intragranular energy, low temperature required for carbothermal reduction reaction, high conversion rate, etc.

Method used

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  • A method for preparing Aln nano-powder by plasma-assisted high-energy ball milling

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Experimental program
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Effect test

Embodiment 1

[0030] Weigh 150g of alumina with a purity of 99.99% and a particle size of 20um. According to the ratio of ball to material ratio of 50:1, put it into a cleaned high-energy ball mill. Under the protection of nitrogen, it is cooled by circulating water and the peak AC voltage is 45kV. , Frequency 8000Hz, ball milling 0-40h, high-energy ball mill rotation 1400rpm, the temperature of the high-energy ball mill tank during the ball milling process is controlled below 50 ℃.

[0031] The ball-milled alumina and carbon black are mixed in a mass ratio of 1:0.6 and put into a high-temperature heating furnace, and the reaction temperature is 1100-1600°C. The holding time was 4h, the atmosphere was circulating nitrogen, and the gas flow was 100ml / min. Then naturally cooled to room temperature.

[0032] After the reaction at different temperatures, put the powder into a clean crucible, and put it into a muffle furnace and heat it in the air at 1000°C, hold it for 4 hours, and then slowly...

Embodiment 2

[0033] Embodiment 2 is the embodiment of adding carbon black during reaction:

[0034] Weigh 150g of alumina with a purity of 99.99%, mix alumina and carbon black at a mass ratio of 1:1, and put it into a cleaned ball mill in a ball-to-material ratio of 50:1. Under the protection of nitrogen, circulate Water cooling, AC peak voltage 45kV, frequency 8000Hz, ball mill 0-40h, ball mill revolution 1400rpm, the temperature of the ball mill tank during the ball milling process is controlled below 50 ℃.

[0035] The ball-milled alumina and carbon black mixed powder is put into a high-temperature heating furnace, and the reaction temperature is 1100-1600 °C. The holding time was 4h, the atmosphere was circulating nitrogen, and the gas flow was 100ml / min. Then naturally cooled to room temperature.

[0036] After the reaction at different temperatures, put the powder into a clean crucible, and put it into a muffle furnace and heat it in the air at 1000°C, hold it for 4 hours, and then...

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Abstract

The invention relates to a method for preparing AlN nanopowder by adopting high-energy ball milling under assistance of plasma and belongs to the technical field of nanometer preparation. According to the method, a bipolar nanosecond-level high-voltage marrow-pulse power supply or an alternating current power supply is taken as driving source under barometric pressure, dielectric barrier discharge plasma is obtained in nitrogen or mixed gas of the nitrogen and argon so as to assist the high-energy ball milling to prepare the AlN nanopowder. The method has the advantages that the operation is simple, the cost is low, the grain size of the AlN nanopowder is smaller than that of aluminum nitride prepared by only adopting ball milling, the malposition defect is large, the internal energy of the grain is high, the required temperature of carbon thermal reduction reaction is low, the conversion rate is high, and the like.

Description

technical field [0001] A method for preparing AlN nano powder by plasma-assisted high-energy ball milling belongs to the technical field of nano preparation. The invention relates to a technical method for preparing AlN nano-powder by utilizing dielectric barrier discharge plasma-assisted high-energy ball milling under atmospheric pressure. Specifically, a bipolar nanosecond high-voltage narrow pulse power supply or an AC power supply is used as a driving source, and a dielectric barrier discharge plasma is obtained in a mixed gas of nitrogen or nitrogen and argon to assist high-energy ball milling to prepare AlN nanopowders. technical background [0002] Aluminum nitride (AlN) is a new type of functional ceramic material with a series of excellent properties such as good thermal conductivity, reliable electrical insulation, low dielectric loss and dielectric constant, and a thermal expansion coefficient close to silicon. It is considered to be an ideal material for highly ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B02C21/00C01B21/072B82Y30/00
Inventor 王文春刘志杰杨德正王森张宝剑戴乐阳
Owner DALIAN UNIV OF TECH
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