Method for preparing porous ceramic by using tertiary butanol-based freezing sublimation method

A technology of porous ceramics and tert-butanol, applied in the field of porous ceramics, can solve the problems of difficulty in increasing porosity and insufficient application range, and achieve the effects of controllable porosity, strong applicability and uniform pore distribution

Inactive Publication Date: 2012-07-04
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for preparing porous ceramics with tert-butanol-based freeze-sublimation method, which solves the problems of insufficient scope of application and difficulty in improving porosity in the prior art, and prepares porous ceramics with straight hole morphology. and further increased the porosity of porous ceramics

Method used

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  • Method for preparing porous ceramic by using tertiary butanol-based freezing sublimation method
  • Method for preparing porous ceramic by using tertiary butanol-based freezing sublimation method
  • Method for preparing porous ceramic by using tertiary butanol-based freezing sublimation method

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Experimental program
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Effect test

Embodiment 1

[0028] The raw material is Al with a particle size of about 400 mesh 2 o 3 39.7 grams of powder, 31.6 grams of tert-butanol, 0.397 grams of citric acid and 0.200 grams of polyvinyl butyral, ball milled for 10 hours, poured the dispersed slurry into a polyethylene mold, the temperature at the bottom of the mold was minus 5 ° C, and The temperature at the top is room temperature (20-30°C), the freezing time is 10 minutes, demolded, sublimated for 24 hours under the condition of water circulation pump suction and filtration (pressure is about 0.098MPa), and then kept at 1500°C in an air furnace for 1 hour. The porous ceramic material is synthesized, and the obtained porous ceramic pores are in the shape of straight pores, with a diameter of 20-60 μm and a porosity of 66%. The corresponding scanned photos are listed in the attached figure 1 superior.

Embodiment 2

[0030] The raw material is Al with a particle size of about 400 mesh 2 o 3 29.9 grams of powder, 33.6 grams of tert-butanol, 0.297 grams of citric acid and 0.161 grams of polyvinyl butyral, ball milled for 15 hours, poured the dispersed slurry into a polyethylene mold, the temperature at the bottom of the mold was minus 3 ° C, and The top temperature is room temperature (20-30°C), the freezing time is 10 minutes, demolded, sublimated under the condition of water circulation pump suction and filtration (pressure is about 0.098MPa) for 48 hours, and then kept at 1400°C in an air furnace for 1 hour. The porous ceramic material is synthesized, and the obtained porous ceramic pores are in the shape of straight pores, the pore diameter is 50-80 μm, and the porosity can reach 72%. The corresponding scanned photos are listed in the attached figure 2 superior.

Embodiment 3

[0032] The raw material is Al with a particle size of about 400 mesh 2 o 3 Powder 19.85 grams, tert-butanol 35.55 grams, citric acid. 0.199 grams and 0.101 grams of polyvinyl butyral, ball milled for 12 hours, pour the dispersed slurry into a polyethylene mold, the temperature at the bottom of the mold is minus 6°C, and the temperature at the top is room temperature (20-30°C). Freeze for 10 minutes, remove the mold, sublimate for 64 hours under the condition of water circulation pump suction and filtration (pressure is about 0.098MPa), and then keep warm at 1500°C for 1 hour in an air furnace to synthesize porous ceramic materials. The obtained porous ceramic pores are straight Pore ​​morphology, the pore diameter ranges from 50 to 100 μm, and the porosity is as high as 84.9%. The relationship between solid content and porosity is shown in the appendix image 3 On the other hand, the porosity increases with the decrease of solid content.

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Abstract

The invention relates to the field of porous ceramics, in particular to a method for preparing a porous ceramic by using a tertiary butanol-based freezing sublimation method. The method disclosed by the invention basically has no restriction to an oxide material system and is generally suitable for engineering ceramics. The method comprises the following steps of: with oxide ceramic powder as a raw material, tertiary butanol as a solvent, citric acid as a dispersing agent and polyvinyl butyral as a binding agent, carrying out ball grinding on the raw material for 5-50h, pouring the uniformly-dispersed raw material into a polyethylene mold of which the bottom temperature is above 0 DEG C and the top temperature is room temperature, and cooling for 5min-2h; and demolding, then sublimating for 24-27h by using a water circulating pump under the condition of suction filtering, and heating to 1200-1600 DEG C in an air furnace and preserving the temperature for 5min-2h. According to the method disclosed by the invention, slurry of an organic system is prepared under the room temperature; and the obtained porous ceramic is distributed with directional holes, wherein the directional holes are polygonal holes and have the size distribution of below 100 microns and the longitudinal lengths of reaching millimeter-scale. According to the method disclosed by the invention, the porosity can be controlled by adjusting the solid content, and the porous ceramic material with ultrahigh porosity (more than 80 percent) can be prepared.

Description

technical field [0001] The invention relates to the field of porous ceramics, in particular to a method for preparing porous ceramics by a tert-butanol-based freeze-sublimation method. Background technique [0002] Porous ceramics refer to new ceramic materials with a certain size and number of pore structures. During the process of material molding and high-temperature sintering, a large number of interconnected or closed pores are formed inside. Porous ceramics have uniformly distributed micropores or holes, high porosity, small bulk density, large specific surface area and unique physical surface properties, and have selective permeability, energy absorption or damping properties for liquid and gas media. Material-specific high temperature resistance, corrosion resistance, high chemical stability and dimensional stability. Therefore, porous ceramics, a green material, can be widely used in many aspects such as gas or liquid filtration, purification and separation, chemi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B38/00
Inventor 周延春李端阳李美栓陈继新王晓辉王京阳
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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