Preparation method of alpha-silicon nitride powder

The technology of silicon nitride powder and powder is applied in the field of preparation of α-silicon nitride powder, which can solve problems such as affecting the formation of silicon nitride crystal grains, and achieve low production cost, high powder purity and easy control. Effect

Inactive Publication Date: 2019-07-05
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the presence of oxygen in the raw material will affect the formation of silicon nitride grains, how to avoid the introduction of oxygen and remove oxygen is a difficult problem

Method used

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  • Preparation method of alpha-silicon nitride powder
  • Preparation method of alpha-silicon nitride powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1), Cr 2 o 3 Weigh the raw materials with Si powder according to the mass ratio of 2.5:97.5, and dope 2.5wt% Cr 2 o 3 The silicon powder of the powder is ball-milled, and the ball-milled powder is put into a silicon nitride ball mill tank, and silicon nitride balls and alcohol are added, wherein the powder: ball: alcohol mass ratio is 1:3:1.5. Put it into a planetary ball mill for ball milling, the rotating speed is 300r / min, and the ball milling time is 4h.

[0037] 2), the above ball milled doped 2.5wt% Cr 2 o 3 The silicon powder was suction filtered to remove the alcohol in the silicon powder; after that, the above filtered powder was dried in a vacuum drying oven to remove residual alcohol at a temperature of 40°C and a drying time of 4 hours. The above-mentioned vacuum-dried sample was ground and passed through a 40-mesh sieve to obtain a powder with uniform particles for subsequent nitriding experiments.

[0038] 3), the doped 2.5wt% Cr after above-mentione...

Embodiment 2

[0040] 1), Cr 2 o 3 Weigh the raw materials with Si powder according to the mass ratio of 2.5:97.5, and dope 2.5wt% Cr 2 o 3 The silicon powder of the powder is ball milled, and the ball milled powder is put into a silicon nitride ball mill tank, and silicon nitride balls and alcohol are added, wherein the powder: ball: alcohol mass ratio is 1:6:1.5. Put it into a planetary ball mill for ball milling, the rotating speed is 400r / min, and the ball milling time is 2h.

[0041]2), the above ball milled doped 2.5wt% Cr 2 o 3 The silicon powder was suction filtered to remove the alcohol in the silicon powder; after that, the above filtered powder was dried in a vacuum drying oven to remove residual alcohol at a temperature of 80°C and a drying time of 2 hours. The above-mentioned vacuum-dried sample was ground and passed through a 40-mesh sieve to obtain a powder with uniform particles for subsequent nitriding experiments.

[0042] 3), the doped 2.5wt% Cr after above-mentioned...

Embodiment 3

[0044] 1), Cr 2 o 3 Weigh the raw materials with Si powder according to the mass ratio of 2.5:97.5, and dope 2.5wt% Cr 2 o 3 The silicon powder of the powder is ball-milled, and the ball-milled powder is put into a silicon nitride ball mill tank, and silicon nitride balls and alcohol are added, wherein the powder: ball: alcohol mass ratio is 1:4:1.5. Put it into a planetary ball mill for ball milling, the rotating speed is 400r / min, and the ball milling time is 2h.

[0045] 2), the above ball milled doped 2.5wt% Cr 2 o 3 The silicon powder was suction filtered to remove the alcohol in the silicon powder; after that, the above filtered powder was dried in a vacuum drying oven to remove residual alcohol at a temperature of 80°C and a drying time of 2 hours. The above-mentioned vacuum-dried samples were ground and passed through a 70-mesh sieve to obtain a powder with uniform particles for subsequent nitriding experiments.

[0046] 3), the doped 2.5wt% Cr after above-mentio...

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Abstract

The invention discloses a preparation method of alpha-silicon nitride powder, which comprises the following steps: carrying out ball milling on silicon powder doped with Cr2O3 powder, adding a siliconnitride grinding ball and alcohol; putting the silicon powder into a ball mill for ball milling, carrying out suction filtration on the ball milled Cr2O3 silicon powder, and removing the alcohol in the silicon powder; drying the filtered powder in a vacuum drying oven, and removing residual alcohol; grinding and sieving a sample subjected to vacuum drying to obtain powder with uniform particles;putting the ground silicon powder doped with Cr2O3 into a high-temperature tubular furnace, vacuumizing, introducing a nitrogen-hydrogen mixed gas, raising the temperature to 800 DEG C at less than orequal to 5 DEG C/min, and raising the temperature to 1300-1400 DEG C/min, keeping the temperature for 2-4 hours to obtain the silicon nitride powder. The preparation method has the advantages of lownitriding temperature, low cost and short nitriding period, wherein the prepared alpha-Si3N4 phase is as high as 96 wt% in the prepared power, and the particle size is small, and part of the Si3N4 phase is fibrous.

Description

technical field [0001] The invention relates to the technical field of ceramic materials, in particular to an α-silicon nitride (α-Si 3 N 4 ) powder preparation method. Background technique [0002] Silicon nitride (Si 3 N 4 ) Ceramic material, as a traditional structural ceramic material, has many excellent physical and chemical properties, high hardness, high strength, good fracture toughness, high temperature stability, chemical stability and thermal shock resistance, and can be used as bearing, turbine Rotors, radomes, etc., are widely used in automobiles, metallurgy, aerospace and other fields. Si 3 N 4 Due to its high mechanical properties and high theoretical thermal conductivity, ceramics are considered to be one of the potential substitute materials for ceramic substrates in electronic packaging. Si 3 N 4 Nanowires have photoluminescent properties and are suitable for high-temperature environments and radiation environments. [0003] However, its applicati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/068C04B35/584C04B35/626
CPCC01B21/0682C04B35/62675C04B35/584C01P2006/80C01P2004/61C01P2004/62C04B2235/5436C04B2235/5445C04B2235/526
Inventor 杨德安高春兰王硕曹利生
Owner TIANJIN UNIV
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