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A method for preparing high-purity silicon nitride powder by liquid-phase assisted combustion synthesis

A silicon nitride powder, auxiliary combustion technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of impurity residues and harm to the health of producers, and achieve high production efficiency, energy saving, and rapid synthesis reaction. Effect

Active Publication Date: 2021-05-28
QINGDAO CUP NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the silicon nitride powder prepared by the commercialized combustion synthesis method needs to use a large amount of chlorine and fluorine-containing ammonium salts as additives in the preparation process, and there are a large amount of impurities in the product, and a large amount of impurities will be produced during production. HCl, HF and other gases that are extremely harmful to the human body seriously endanger the health of producers

Method used

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  • A method for preparing high-purity silicon nitride powder by liquid-phase assisted combustion synthesis
  • A method for preparing high-purity silicon nitride powder by liquid-phase assisted combustion synthesis
  • A method for preparing high-purity silicon nitride powder by liquid-phase assisted combustion synthesis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Weigh raw materials according to weight ratio: 200 mesh silicon powder is 30%, and silicon nitride (average particle size 2 μm) is 70%.

[0030] (2) After mixing the raw materials with alcohol, use silicon nitride balls as the medium, ball mill on a rolling ball mill for 1 hour, and then vacuum dry at 80°C.

[0031] (3) Mix the dried raw material powder with alcohol that accounts for 20% of the weight ratio of the raw material powder in a high-speed mixer. Then mix for 1 min.

[0032] (4) The raw material powder is directly loaded into a porous graphite boat and placed in a combustion synthesis device. After vacuuming, fill it with 1MPa high-purity nitrogen. Use titanium powder as the ignition agent to induce combustion synthesis reaction. After the combustion reaction is over, the gas in the device is released, and at the same time, when the circulating water is cooled to below 40°C, the door of the chamber is opened to take out the reaction product.

[0033] T...

Embodiment 2

[0035] (1) Weigh raw materials according to weight ratio: 200 mesh silicon powder is 70%, silicon nitride (average particle size 2 μm) is 30%.

[0036] (2) After the raw materials are mixed with alcohol, they are ball-milled on a rolling ball mill for 1 h with silicon nitride balls as the medium, and then vacuum-dried at 80°C.

[0037] (3) Mix the dried raw material powder with 0.5% alcohol in the weight ratio of the raw material powder in a high-speed mixer. During the mixing process, the alcohol is added to the raw material at one time and mixed for 5 minutes.

[0038] (3) The raw material powder is directly loaded into a porous graphite boat and placed in a combustion synthesis device. After vacuuming, fill it with 4.5MPa high-purity nitrogen. Use titanium powder as the ignition agent to induce combustion synthesis reaction. After the combustion reaction is over, the gas in the device is released, and at the same time, when the circulating water is cooled to below 40°C, t...

Embodiment 3

[0041] (1) Weigh raw materials according to weight ratio: 100 mesh silicon powder is 50%, silicon nitride (average particle size 2 μm) is 50%.

[0042] (2) After the raw materials are mixed with alcohol, they are ball-milled on a rolling ball mill for 1 h with silicon nitride balls as the medium, and then vacuum-dried at 80°C.

[0043] (3) Mix the dried raw material powder with 10% alcohol in a high-speed mixer in the weight ratio of the raw material powder. During the mixing process, the alcohol is mixed into the raw material in a small amount and multiple times. 1min.

[0044] (4) The raw material powder is directly loaded into a porous graphite boat and placed in a combustion synthesis device. After vacuuming, fill it with 1MPa high-purity nitrogen. Use titanium powder as the ignition agent to induce combustion synthesis reaction. After the combustion reaction is over, the gas in the device is released, and at the same time, when the circulating water is cooled to below ...

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Abstract

The invention discloses a method for synthesizing high-purity silicon nitride powder by liquid-phase assisted combustion and belongs to the technical field of inorganic non-metallic powder preparation. The specific steps of the present invention are: mixing silicon powder and silicon nitride diluent in proportion, ball milling the mixture to make it evenly mixed, and then drying to obtain the raw material powder; In the reaction device, the reaction is induced under a specific pressure to obtain high-purity silicon nitride powder. The synthesis process of the present invention does not use any additional additives, has the characteristics of no pollution and no toxicity, and the synthesized silicon nitride powder has good crystallinity and high purity, and no complicated post-treatment process is required.

Description

technical field [0001] The invention belongs to the technical field of inorganic non-metallic powder preparation, and in particular relates to a method for preparing high-purity silicon nitride powder through liquid-phase assisted combustion synthesis. Background technique [0002] Silicon nitride ceramics have many excellent properties such as low density, high thermal conductivity, high hardness, good thermal stability and chemical stability, and are the most excellent comprehensive performance materials in the family of structural ceramics. Widely used in ceramic engines, cutting tools, heat conduction substrates and other fields. Silicon nitride powder is its main raw material, and its important position can be seen. The combustion synthesis method has been widely concerned and valued due to its energy saving, high efficiency and many other advantages. However, the silicon nitride powder prepared by the commercialized combustion synthesis method needs to use a large am...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/068C04B35/591C04B35/626
CPCC01B21/0682C01P2002/72C01P2004/61C01P2006/80C04B35/591C04B35/626C04B35/62615C04B35/6268
Inventor 张杰刘光华崔巍邹艺峰成会明
Owner QINGDAO CUP NEW MATERIALS CO LTD
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