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
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[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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