Method for in-situ synthesis of Si3N4-Si2N2O-TiN ternary compound powder

A ternary composite and in-situ synthesis technology, applied in the field of composite ceramic materials, can solve the problems of difficult dispersion, non-uniform and fine distribution, easy agglomeration, etc., and achieve the effects of improving ceramic performance, promoting high performance, and accelerating nitriding

Active Publication Date: 2016-06-01
吉林长玉特陶新材料技术股份有限公司
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

Both exist SiO 2 and TiO 2 Easy to agglomerate and difficult to disperse problems, leading to Si 2 N 2 O and TiN phases cannot be in Si 3 N 4 Uniform and fine distribution in ceramics

Method used

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  • Method for in-situ synthesis of Si3N4-Si2N2O-TiN ternary compound powder
  • Method for in-situ synthesis of Si3N4-Si2N2O-TiN ternary compound powder
  • Method for in-situ synthesis of Si3N4-Si2N2O-TiN ternary compound powder

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Experimental program
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Embodiment 1

[0032] In situ synthesis of Si of the present invention 3 N 4 -Si 2 N 2 The method for O-TiN ternary composite powder, comprises the steps:

[0033] (1) Using Si powder and butyl titanate as raw materials, the mass fraction of Si powder is 73%, and the mass fraction of butyl titanate is 27%. With ethanol as solvent, Si 3 N 4 The ball is a ball milling medium, mixed on a planetary ball mill for 12 hours, after mixing and drying, a uniformly mixed Si-TiO 2 Composite powder, wherein the mass fraction of Si powder is 92%, TiO 2 The mass fraction is 8%.

[0034] (2) Si-TiO 2 Composite powder dry pressing to obtain Si-TiO 2 Green body, Si-TiO 2 Put the green body into a graphite crucible, raise the temperature to 1400°C at a heating rate of 10°C / min, and keep it warm for 2 hours. The atmosphere of the whole process is 1atm nitrogen, and Si is synthesized in situ. 3 N 4 -Si 2 N 2 O-TiN ternary composite powder.

[0035] The Si prepared in this example 3 N 4 -Si 2 N 2 ...

Embodiment 2

[0037] The in-situ synthesis of Si in this embodiment 3 N 4 -Si 2 N 2 The method of O-TiN ternary composite powder is as follows:

[0038] According to the mass fraction of Si powder is 82%, the mass fraction of butyl titanate is 18%, with ethanol as solvent, Si 3 N 4 The ball is a ball milling medium, mixed on a planetary ball mill for 12 hours, mixed and dried to obtain Si-TiO 2 Composite powder, where Si and TiO 2 The mass fraction ratio is 95%: 5%, and Si is synthesized in situ according to the method of Example 1 3 N 4 -Si 2 N 2 O-TiN ternary composite powder, in which the temperature is raised to 1400 ° C for 2 hours. Prepared Si 3 N 4 -Si 2 N 2 O-TiN ternary composite powder, Si 3 N 4 、Si 2 N 2 O and TiN particle sizes are 3.7μnm, 3.8μnm, 0.7μnm, Si 3 N 4 : Si 2 N 2 O: TiN mass fraction ratio is 89.9%: 7.7%: 2.4%, and Si 2 N 2 O and TiN are uniformly distributed on Si 3 N 4 middle.

Embodiment 3

[0040] The in-situ synthesis of Si in this embodiment 3 N 4 -Si 2 N 2 The method of O-TiN ternary composite powder is as follows:

[0041] According to Si powder mass fraction of 92%, butyl titanate mass fraction of 8% for batching, with ethanol as solvent, Si 3 N 4 The ball is a ball milling medium, mixed on a planetary ball mill for 12 hours, mixed and dried to obtain Si-TiO 2 Composite powder, where Si and TiO 2 The mass fraction ratio is 98%: 2%, and Si is synthesized in situ according to the method of Example 1 3 N 4 -Si 2 N 2 O-TiN ternary composite powder, in which the temperature is raised to 1400 ° C for 2 hours. Prepared Si 3 N 4 -Si 2 N 2 O-TiN ternary composite powder, Si 3 N 4 、Si 2 N 2 O and TiN particle sizes are 3.1μnm, 3μnm, 0.5μnm, Si 3 N 4 : Si 2 N 2 O: TiN mass fraction ratio is 96%: 3%: 1%, and Si 2 N 2 O and TiN are uniformly distributed on Si 3 N 4 middle.

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Abstract

The invention discloses a method for in-situ synthesis of Si3N4-Si2N2O-TiN ternary compound powder. The method comprises the steps that Si powder and butyl titanate are adopted as raw materials, Si-TiO2 compound powder is obtained through mixing and drying according to the mass ratio that Si: butyl titanate is (48%-96%):(4%-52%), and the mass ratio of Si to TiO2 is (80%-99%):(1%-20%); the compound powder is subjected to dry pressing, and placed in an atmosphere oven to be nitrided, the nitriding temperature ranges from 1,300 DEG C to 1,450 DEG C, the time ranges from 0.5 h to 20 h, and the nitriding process atmosphere is nitrogen of 1 atm; the Si3N4-Si2N2O-TiN ternary compound powder is synthesized through an in-situ reaction, and the mass ratio of Si3N4 to Si2N2O to TiN is (57%-98%):(1.5%-33%):(0.5%-10%). Nitriding of the Si powder is accelerated, forming of a high-performance Si2N2O phase is promoted, an evenly-distributed TiN phase with the small particle size is formed, and the performance of Si3N4 ceramic is remarkably improved.

Description

technical field [0001] The invention relates to the field of composite ceramic materials, and specifically discloses an in-situ synthesized Si 3 N 4 -Si 2 N 2 O-TiN ternary composite powder method. Background technique [0002] As a structural ceramic, Si 3 N 4 Ceramics have excellent properties such as high toughness, high temperature resistance, and high thermal conductivity, but low high temperature stability, oxidation resistance, and wear resistance. with Si 3 N 4 Compared to Si 2 N 2 O has high high temperature stability and oxidation resistance, and TiN has high hardness, wear resistance and electrical conductivity. Therefore, Si 2 N 2 O and TiN as the second phase, added to the Si 3 N 4 Ceramics can significantly improve its high temperature stability, wear resistance, thermal shock resistance, and electrical conductivity. [0003] At present, mainly by adding SiO to the raw material 2 phase, in situ reaction to generate Si 2 N 2 O phase; by adding ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/591C04B35/626
CPCC04B35/591C04B35/62645C04B2235/3865C04B2235/3873C04B2235/428C04B2235/46
Inventor 郭伟明陈珊璐黄楚云林华泰
Owner 吉林长玉特陶新材料技术股份有限公司
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