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Forming method for preparing Si3N4 porous ceramic through tertiary butyl alcohol (TBA)-based gel casting method

A technology of porous ceramics and a molding method, applied in the field of porous ceramics, can solve the problems of no retrieval, low strength of oxide ceramic products, etc., and achieve the effects of increasing porosity, solving easy deformation and cracking, and low surface tension

Inactive Publication Date: 2012-02-08
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Literature Ceramics With Ultra-Low Density Fabricated by Gel-casting: An Unconventional Vie (Ruifeng Chen, Yong Huang etc, J.Am.Ceram.Soc.90[11]3424-3429(2007)), prepared a volume fraction of 5 -15% Al 2 o 3 Ceramics, in which the porosity is 60%-92%, and the strength is 10-50Mpa; literature Porous yttria stabilized zirconia ceramics with ultra-low thermal conductivity (Liang Fa Hu, Chang An Wang, Yong Huang, J Mater Sci (2010) 45: 3242 -3246) with TBA as solvent, ZrO with high porosity (52-76%) and uniform pore size distribution (0.7-1.8 μm) was prepared by gel injection molding 2 Ceramics, the above-mentioned reports all use TBA-based gel injection molding to prepare oxide ceramics, and the formability of oxide ceramics is relatively good, but the strength of oxide ceramic products is relatively low
[0007] At present, there is no search for the preparation of porous Si by gel injection molding using TBA as a solvent. 3 N 4 Literature and published invention patents of ceramics

Method used

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  • Forming method for preparing Si3N4 porous ceramic through tertiary butyl alcohol (TBA)-based gel casting method
  • Forming method for preparing Si3N4 porous ceramic through tertiary butyl alcohol (TBA)-based gel casting method
  • Forming method for preparing Si3N4 porous ceramic through tertiary butyl alcohol (TBA)-based gel casting method

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Experimental program
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Effect test

Embodiment 1

[0026] The process steps are as follows:

[0027] (1) Ball milling: take 20wt% Si according to the design composition 3 N 4 After powder and 80wt% TBA powder, add 15% organic matter, wherein the ratio of AM and MBAM is 4:1. Then fully mix uniformly, use agate balls as grinding balls, material powder: agate balls=1:1 (mass ratio), place in a nylon tank and utilize a rolling ball mill to mix materials for 12h;

[0028] (2) Molding: Pour the ball-milled slurry into a polytetrafluoroethylene mold, place it in a water bath at 30-65°C for 35-60 minutes, and then demould

[0029] (3) Drying: put the demoulded green body on a glass plate, and dry it for 24 hours under natural ventilation;

[0030] (4) Debinding: slow debinding in an air furnace, the highest debinding temperature is 560°C, and the heating rate is 0.2°C / min;

[0031] (5) High temperature sintering: after nitriding, the sample is sintered at high temperature, the sintering temperature is 1700°C, and the holding time ...

Embodiment 2

[0034] (1) Ball milling: take 30wt% Si according to the design composition 3 N 4After powder and 70wt% TBA powder, add 15% organic matter, wherein the ratio of AM and MBAM is 4:1. Then fully mix uniformly, use agate balls as grinding balls, material powder: agate balls=1:1 (mass ratio), place in a nylon tank and utilize a rolling ball mill to mix materials for 12h;

[0035] (2) Forming: Pour the ball-milled slurry into a polytetrafluoroethylene mold, place it in a water bath at 30-65°C for 35-60 minutes to form; then demould;

[0036] (3) Drying: put the demoulded green body on a glass plate, and dry it for 24 hours under natural ventilation;

[0037] (4) Degumming: slowly degumming in the air path, the highest degumming temperature is 560°C, and the heating rate is 0.2°C / min;

[0038] (5) High temperature sintering: after nitriding, the sample is sintered at high temperature, the sintering temperature is 1700°C, and the holding time is 1.5h;

[0039] The product of the pr...

Embodiment 3

[0041] (1) Ball milling: take 40wt% Si according to the design composition 3 N 4 After powder and 60wt% TBA powder, add 15% organic matter, wherein the ratio of AM and MBAM is 4:1. Then fully mix uniformly, use agate balls as grinding balls, material powder: agate balls=1:1 (mass ratio), place in a nylon tank and utilize a rolling ball mill to mix materials for 12h;

[0042] (2) Forming: Pour the ball-milled slurry into a polytetrafluoroethylene mold, place it in a water bath at 30-65°C for 35-60 minutes to form; then demould;

[0043] (3) Drying: put the demoulded green body on a glass plate, and dry it for 24 hours under natural ventilation;

[0044] (4) Degumming: slowly degumming in the air path, the highest degumming temperature is 560°C, and the heating rate is 0.2°C / min

[0045] (5) High temperature sintering: after nitriding, the sample is sintered at high temperature, the sintering temperature is 1700°C, and the holding time is 1.5h;

[0046] The product of the pr...

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Abstract

The invention discloses a forming method for preparing Si3N4 porous ceramic through a tertiary butyl alcohol (TBA)-based gel casting method, belonging to the field of porous ceramic. In the method, TBA is used as a new solvent instead of the solvent water in the traditional water-based gel casting forming. The method comprises the following steps: dissolving acrylamide, N,N'-methylene bisacrylamide and polyvinyl pyrrolidone in the TBA, and preparing into a premixed liquid; then adding Si3N4, Al2O3 and Y2O3, and carrying out ball milling for 12 hours; and carrying out forming, drying, binder removal, sintering and other procedures to prepare high-porosity high-strength silicon nitride porous ceramic, wherein the porosity of the ultimately prepared Si3N4 porous ceramic ranges between 40% and 75%, and the strength is 40-140 Mpa. The method has the following advantages: (1) the problem of Si3N4 hydrolysis in the conventional water-based gel casting forming process is avoided; and (2) the problem of high cracking possibility during the forming and drying of water-based gel casting is solved, and the forming and drying process of gel casting is simplified.

Description

technical field [0001] The present invention relates to a kind of tert-butanol base (TBA) gel casting method to prepare Si 3 N 4 The invention relates to a technique of porous ceramics, which belongs to the field of porous ceramics. Background technique [0002] Porous ceramics is a kind of ceramic material with gas phase as the main phase. Compared with other porous materials, it has the advantages of high temperature resistance, corrosion resistance and thermal shock resistance. It has wide applications in metallurgy, chemical industry, biology, aerospace and other fields. prospect. All countries in the world have invested a lot of manpower, material resources, and financial resources in the research of such materials, and have made great progress. [0003] Silicon nitride ceramics are one of the materials with the best comprehensive performance in structural ceramics. In addition to the advantages of ordinary ceramic materials such as high strength, high elastic modul...

Claims

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Application Information

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IPC IPC(8): C04B38/00C04B35/624C04B35/584
Inventor 王红洁李刘媛乔冠军杨建锋
Owner XI AN JIAOTONG UNIV
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