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A kind of preparation method of conductive network structure si3n4 ceramics

A technology of network structure and ceramics, which is applied in the field of preparation of Si3N4 ceramics with conductive network structure, can solve the problems of long holding time, high nitrogen pressure, and long nitriding time of Si powder, etc., and achieves relaxation of densification conditions, improvement of wear resistance, The effect of accelerating the nitriding speed

Active Publication Date: 2018-06-26
吉林长玉特陶新材料技术股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Preparation of Si by reactive pressure sintering of Si powder 3 N 4 There are two main problems in ceramics: (1) The nitriding time of Si powder is long, and it needs to be kept at 1400°C for 8 hours; (2) Si powder 3 N 4 Densification conditions are too harsh, high nitrogen pressure (10atm), high sintering temperature (1900°C), long holding time (12h)
In addition, Si 3 N 4 Because of its high hardness and high brittleness, ceramics are difficult to process, especially they cannot be used for EDM to form workpieces with complex shapes, thus limiting their industrial application
[0004] If in Si 3 N 4 Ceramics are added to the conductive network structure. The traditional method is to directly mix the conductive phase, such as TiN or TiCN, etc., and there are the following problems: 1) It needs a large amount of mixing to achieve a good conductive effect, usually about 40%, and the existing technology is difficult. A network-like distribution is formed when less conductive phases are introduced; 2) Adding too much conductive phase is not conducive to the sintering and densification of ceramics, and ceramics are prone to agglomeration, resulting in uneven distribution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0034] A conductive network structure Si 3 N 4 The preparation method of pottery, comprises the following steps:

[0035] 1) Using Si powder as raw material, Al 2 o 3 -Re 2 o 3 As a sintering aid, Si-Al can be obtained after mixing, ball milling and drying 2 o 3 -Re 2 o 3 Mixed powder; wherein Re is a rare earth element;

[0036] 2) Si-Al obtained in step 1) 2 o 3 -Re 2 o 3 The mixed powder is finalized, pre-fired under a nitrogen atmosphere, and the pre-fired green body is placed in MO 2 Soak in the sol for 0.5-24h, after drying, carry out secondary sintering under nitrogen atmosphere to prepare Si with conductive network structure 3 N 4 ceramics.

[0037] Preferably, the rare earth element Re includes Sc, Y, La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu.

[0038] More preferably, the rare earth element Re is Y, Yb, Gd, Ce, Eu.

[0039] More preferably, the rare earth element Re is Y.

[0040] Preferably, the purity of Si powder is 95% to 100%,...

Embodiment 1

[0059] A conductive network structure Si 3 N 4 The preparation method of pottery, comprises the following steps:

[0060] In the present invention, Si powder (particle size2 powder (particle size 2 o 3 Powder (99.9% pure) and Y 2 o 3 Powder (99.9% purity) is an additive.

[0061] Accurately weigh the raw materials of each component according to the following mass percentages: including 90% Si powder, 10% Al 2 o 3 -Y 2 o 3 (where Al 2 o 3 : Y 2 o 3 The mass percentage is 55%: 45%), with ethanol as solvent, with Si 3 N 4 The ball is the ball milling medium, mixed on a planetary ball mill for 8 hours, after mixing and drying, a uniformly mixed Si-Al 2 o 3 -Y 2 o 3 Mix powder. Si-Al 2 o 3 -Re 2 o 3 The mixed powder is put into the mold, and after the green body is obtained by dry pressing, the temperature is raised to 1200°C at 20°C / min for pre-sintering, and the temperature is kept for 2 hours. The sintering atmosphere during the whole process is nitrogen. ...

Embodiment 2

[0064] Accurately weigh the raw materials of each component according to the following mass percentages: including 80% Si powder, 20% Al 2 o 3 -Yb 2 o 3 (where Al 2 o 3 : Yb 2 o 3 The mass percentage is 60%: 40%). According to the method of Example 1, after pre-fired at 1100 °C for 2 hours under a nitrogen atmosphere, the pre-fired green body was heated in 3mol / L TiO 2 Soaked in the sol for 4h, the secondary sintering process is to first raise the temperature to 1375°C for 4h under nitrogen atmosphere, then raise the temperature to 1900°C for 2h, pressurize 30MPa hot press sintering. Prepared Si 3 N 4 The relative density of the ceramic is 99%, the mass fraction of TiN introduced is 5%, and the electrical conductivity reaches 2000 S m -1 , can be processed into workpieces with complex shapes by EDM, the hardness of the material is 16GPa, and the fracture toughness is 10MPam 1 / 2 , The bending strength is 1000Mpa.

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Abstract

The invention discloses a making method for Si3N4 ceramic of a conductive network structure. The making method comprises the steps that 1, Si powder is used as a raw material, Al2O3-Re2O3 is used as a sintering aid, and mixing, ball-milling and drying are carried out to obtain Si-Al2O3-Re2O3 mixed powder, wherein Re refers to the rare earth element; 2, the Si-Al2O3-Re2O3 mixed powder obtained in the step 1 is shaped and pre-sintered in a nitrogen atmosphere, and a green body obtained after pre-sintering is soaked in MO2 sol for 0.5-24 hours, dried and subjected to secondary sintering in the nitrogen atmosphere to make the Si3N4 ceramic of the conductive network structure. The relative density of the obtained Si3N4 ceramic is larger than 95%, the conductivity reaches 1,000-3,000 Sm-1, the hardness is 8-20 GPa, the breaking tenacity is 6-12 MPa m<1 / 2>, and the bending strength is 800-1,200 MPa. The Si3N4 ceramic can be processed into workpieces in any shape by means of electrical discharge machining, especially workpieces with complicated shapes like ceramic turbine blades, and common Si3N4 ceramic on the market currently does not have the characteristic.

Description

technical field [0001] The invention specifically relates to a conductive network structure Si 3 N 4 Methods of preparation of ceramics. Background technique [0002] Si 3 N 4 Ceramics have excellent properties such as wear resistance and high temperature resistance, and are widely used in high-speed cutting tools and key parts of engines. Usually Si 3 N 4 Ceramics with high purity Si 3 N 4 The powder is prepared by hot pressing and sintering as raw material, the cost is high, and samples with complex shapes cannot be prepared. [0003] In order to reduce costs and prepare complex shapes, Si powder was used as raw material to prepare Si by reactive pressure sintering. 3 N 4 ceramics. On the one hand, the powder preparation and ceramic densification are combined in one step, which significantly reduces the cost; on the other hand, through gas pressure sintering, Si 3 N 4 Preparation of ceramics. However, since the nitriding speed of Si powder is relatively slow,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/584C04B35/622
CPCC04B35/584C04B35/5935C04B35/622C04B2235/3217C04B2235/3224C04B2235/3232C04B2235/3244C04B2235/428C04B2235/658C04B2235/661C04B2235/77C04B2235/96
Inventor 郭伟明吴利翔林华泰
Owner 吉林长玉特陶新材料技术股份有限公司
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