A kind of method for preparing aln ceramic powder by carbothermal reduction nitridation method

A ceramic powder, nitriding technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of high CO concentration, high pressure, hindering the reaction process, etc., to reduce O content, stable performance, The effect of increasing production

Active Publication Date: 2022-07-15
DALIAN MARITIME UNIVERSITY
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Problems solved by technology

It can be seen from the reaction equation that the carbothermal reduction nitriding reaction consumes N 2 The simultaneous generation of 3 times the N 2 The number of moles of CO, that is, the area of ​​the powder layer where the reaction occurs, especially the pressure inside the powder layer is relatively high, and the concentration of CO is relatively high, so that the gas N required for the reaction to proceed 2 Difficult to enter deep into the powder layer, hindering the reaction process

Method used

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  • A kind of method for preparing aln ceramic powder by carbothermal reduction nitridation method
  • A kind of method for preparing aln ceramic powder by carbothermal reduction nitridation method
  • A kind of method for preparing aln ceramic powder by carbothermal reduction nitridation method

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Embodiment 1

[0049] γ-Al with an average particle size of 20nm 2 O 3 AlN ceramic powder was synthesized by carbothermal reduction nitridation method in nitrogen atmosphere using activated carbon as raw material. The main steps include:

[0050] ①Ingredients: Weigh γ-Al according to the carbon content (the mass percentage of activated carbon in the mixed powder) is 36% 2 O 3 Mixed powder with activated carbon, put the weighed powder in a high-energy ball mill tank equipped with alumina balls, and inject deionized water as the ball milling medium (the ratio of ball to material is 10:1, and the ratio of liquid to solid is 4:1) , milled at 300rpm for 5h, and used a spray dryer to dry and granulate the slurry;

[0051] ②Loading and pulse air pressure control: lay graphite paper around and at the bottom of the graphite material box, put the mixed powder obtained in step ① into the above-mentioned graphite material box, the height of the mixed powder is 27mm, and place the graphite material b...

Embodiment 2

[0059] Embodiment 2 According to the method of embodiment 1, the difference is that the furnace pressure lower limit is set to 2.0kPa, the upper limit pressure is set to 4kPa, and the circulation cycle is 4.4min; step 3. heating rate is 5 ℃ / min. The XRD results of the synthesized powders at different positions (upper surface, middle, lower surface and side) of the powder layer are shown in Image 6 , all of which are pure AlN; the oxygen content of the powder is 1.02%; the synthesized AlN ceramic powder has small crystal grains, see Figure 7 (a), the particle morphology after ball milling is shown in Figure 7 (b); The particle size distribution of AlN ceramic powder after ball milling is shown in Figure 8 , the average particle size is about 1 μm.

Embodiment 3

[0061] Embodiment 3 is in accordance with the method of embodiment 1, the difference is that step ③ synthesis temperature is 1650 ℃. The XRD results of the powders synthesized at different positions of the powder layer (upper surface, middle part, lower surface and side surface) are shown in Figure 9 , indicating that the powder phase composition prepared by this method is all pure AlN; the oxygen content of the powder is 0.92%; Figure 10 (a), the particles of the powder after ball milling are fine, and the morphology is shown in Figure 10 (b); The particle size distribution of AlN ceramic powder after ball milling at 210rpm is shown in Figure 11 , the average particle size is about 0.9 μm.

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Abstract

The invention relates to a method for preparing AlN ceramic powder by a carbothermal reduction nitridation method, and belongs to the field of ceramic material preparation. A method for preparing AlN ceramic powder by carbothermal reduction nitridation method, the method uses alumina powder, carbon powder and nitrogen as raw materials in an atmosphere synthesis device, and in the preparation process, continuously or continuously or Nitrogen is introduced intermittently, and the gas pressure in the atmosphere synthesis device is controlled by adjusting the charging rate and the exhaust rate to generate a pressure difference, so that it has the pulse-type characteristics of slow charging and fast discharging, and it changes dynamically in real time in a periodic cycle, and the cycle period is 0.1 ~20min. In the absence of additives, the invention utilizes the air pressure regulation technology to form a pulsed periodic cycle of real-time changing air pressure, promotes the gas exchange inside and outside the powder layer, and can still obtain pure phase AlN under the condition of increasing the thickness of the powder layer, so as to ensure the AlN powder. quality.

Description

technical field [0001] The invention relates to a method for preparing AlN ceramic powder by a carbothermal reduction nitridation method, and belongs to the field of ceramic material preparation. Background technique [0002] AlN has good chemical stability and thermal stability, as well as excellent thermal conductivity, high mechanical strength and low dielectric constant. Its thermal expansion coefficient is close to that of silicon, and it is easily compatible with other semiconductor materials. It is a large-scale integration It is one of the preferred materials for insulating heat dissipation packaging of circuits and semiconductor substrates, and is widely used in the fields of electronic components and optical devices. [0003] High-purity AlN ceramic powder is an essential raw material for the preparation of its high-performance devices. At present, the methods for preparing AlN ceramic powder include carbothermal reduction nitridation method, direct nitridation me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/072
CPCC01B21/0726
Inventor 单英春徐久军徐锦海
Owner DALIAN MARITIME UNIVERSITY
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