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Preparation method of nanometer silicon nitride powder

A silicon nitride powder and nano technology, which is applied in the field of preparation of nano silicon nitride powder, can solve the problems of affecting product quality, uneven mixing, incomplete nitriding, etc., and achieves low cost, good sphericity, and high efficiency. high effect

Active Publication Date: 2020-05-08
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the particle size and impurities of raw materials affect the product quality, especially the density difference between silicon dioxide and carbon source, resulting in uneven mixing and incomplete nitriding

Method used

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  • Preparation method of nanometer silicon nitride powder
  • Preparation method of nanometer silicon nitride powder
  • Preparation method of nanometer silicon nitride powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Weigh 1 mol of tetraethyl orthosilicate, 1 mol of glucose, and 1.5 mol of ammonium nitrate, stir the tetraethyl orthosilicate in the alcohol solution evenly, dissolve the glucose and ammonium nitrate in deionized water completely, and deionized water The volume ratio with alcohol is 2:1;

[0024] 2. Mix and stir the two solutions evenly, heat to 50°C and keep stirring until a viscous slurry is formed;

[0025] 3. Put the slurry into a furnace at 300°C to react for 1 hour, accompanied by flowing nitrogen gas, and the gas flow rate is 0.2 L / min. A mixture of silica and carbon is obtained after the reaction;

[0026] 4. React the obtained mixture of silicon dioxide and carbon at 1450° C. with nitrogen gas for 6 hours to obtain a silicon nitride product.

[0027] 5. The particle size of the silicon nitride powder prepared by this scheme is 60nm.

Embodiment 2

[0029] 1. Weigh 1 mol of tetraethyl orthosilicate, 2 mol of glucose, and 1.5 mol of ammonium nitrate, stir the tetraethyl orthosilicate in the alcohol solution evenly, dissolve the glucose and ammonium nitrate in deionized water completely, and deionized water The volume ratio with alcohol is 2:1;

[0030] 2. Mix and stir the two solutions evenly, heat to 50°C and keep stirring until a viscous slurry is formed;

[0031] 3. Put the slurry into a furnace at 300°C to react for 1 hour, accompanied by flowing nitrogen gas, and the gas flow rate is 0.2 L / min. A mixture of silica and carbon is obtained after the reaction;

[0032] 4. React the obtained mixture of silicon dioxide and carbon at 1450° C. with nitrogen gas for 4 hours to obtain a silicon nitride product.

[0033] 5. The particle size of the silicon nitride powder prepared by this scheme is 50nm.

Embodiment 3

[0035] 1. Weigh 1 mol of tetraethyl orthosilicate, 1 mol of glucose, and 1.5 mol of ammonium nitrate, stir the tetraethyl orthosilicate in the alcohol solution evenly, dissolve the glucose and ammonium nitrate in deionized water completely, and deionized water The volume ratio with alcohol is 2:1;

[0036] 2. Mix and stir the two solutions evenly, heat to 40°C and keep stirring until a viscous slurry is formed;

[0037] 3. Put the slurry into a furnace at 350°C for 1.5 hours, accompanied by flowing argon gas, and the gas flow rate is 0.1 L / min. A mixture of silica and carbon is obtained after the reaction;

[0038] 4. React the obtained mixture of silicon dioxide and carbon at 1400° C. with nitrogen gas for 6 hours to obtain a silicon nitride product.

[0039] 5. The particle size of the silicon nitride powder prepared by this scheme is 70nm.

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Abstract

The invention discloses a preparation method of nanometer silicon nitride powder, and belongs to the technical field of ceramic powder preparation. The preparation method comprises the following steps: (1) preparing a mixed solution from tetraethyl orthosilicate, ammonium nitrate and a water-soluble organic matter according to a certain ratio; (2) heating and stirring the mixed solution at a temperature not higher than 100 DEG C to obtain a viscous slurry; (3) reacting the slurry in a non-oxygen environment of 100-400 DEG C to obtain a precursor; (4) carrying out a reaction on the precursor ina nitrogen atmosphere at 1300-1500 DEG C for 1-10 h to obtain silicon nitride powder; and (5) then removing excess carbon in the air. The method is simple in process, high in efficiency and low in cost, obtained silicon nitride powder particles are good in sphericity degree, and the particle size is smaller than 100 nm.

Description

technical field [0001] The invention belongs to the technical field of ceramic powder preparation, and relates to a preparation method of nanometer silicon nitride powder. Background technique [0002] Silicon nitride is a strong covalent bond compound with high hardness, high strength, small thermal expansion coefficient, self-lubrication, wear resistance, good thermal shock resistance, corrosion resistance, and high temperature oxidation resistance. There are applications in many fields. Silicon nitride has two crystal forms under normal pressure, α-phase silicon nitride and β-phase silicon nitride. At high temperature, the α-phase usually transforms into β-phase, so α-phase silicon nitride is usually used as raw material powder to prepare silicon nitride. ceramics. At present, there are mainly three methods to prepare silicon nitride powder, the direct nitriding method of elemental silicon, the pyrolysis method of silicon imine and the carbothermal reduction method. Th...

Claims

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Application Information

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IPC IPC(8): C01B21/068B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B21/0685C01P2002/72C01P2004/32C01P2004/64
Inventor 王月隆田建军秦明礼吴昊阳贾宝瑞张智睿章林曲选辉
Owner UNIV OF SCI & TECH BEIJING
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