CN105523773A - Method for preparing micro-porous silicon nitride ceramic through gel casting - Google Patents
Method for preparing micro-porous silicon nitride ceramic through gel casting Download PDFInfo
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- CN105523773A CN105523773A CN201510761777.4A CN201510761777A CN105523773A CN 105523773 A CN105523773 A CN 105523773A CN 201510761777 A CN201510761777 A CN 201510761777A CN 105523773 A CN105523773 A CN 105523773A
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Abstract
The invention relates to the technical field of preparation of rare metal materials, specifically to a method for preparing micro-porous silicon nitride ceramic through gel casting. The method comprises the following steps: dissolving polyacrylamide in deionized water, carrying out mechanical stirring for 10 min and then adding monomer, a cross-linking agent and a dispersing agent so as to form a premix solution; adding silicon nitride powder and a sintering aid into the premix solution, adjusting a pH value to 11, carrying out ball milling for 12 h so as to prepare slurry, subjecting the slurry to vacuum degassing, then adding an initiator to remove gas, carrying out injection molding, then carrying out a reaction at 65 DEG C for 40 min so as to allow the slurry to be gelled and cured and then carrying out demolding; carrying out drying at 25 DEG C in an environment with humidity of 98%; and subjecting a dried green body to degreasing, carrying out sintering after degreasing and carrying out heat preservation for 1 h so as to obtain a ceramic sintered body. The micro-porous silicon nitride ceramic prepared by using the method has bending strength of as high as more than 137 MPa, porosity of more than 50%, pore mean diameter of less than 1 [mu]m, uniform pore size distribution and defect-free microstructure.
Description
Technical field
The present invention relates to Rare Metals Materials preparing technical field, be specifically related to a kind of method that gel casting forming prepares micro-porous silicon nitride ceramic.
Background technology
Porous SiN ceramic is as a kind of novel composite ceramic material, except hard, heat-resisting, wear-resisting, corrosion-resistant, the stable advantage such as chemical property, low-k, dielectric loss with general silicon nitride ceramic material, there is again the features such as the uniform perviousness of porous ceramics, larger specific surface area, low density simultaneously.Therefore, porous SiN ceramic can be used as filtration, separation, sound-absorbing, sensitive material and biological ceramics etc., and it is widely used in the industries such as Aeronautics and Astronautics, the energy, oil, chemical industry, environmental protection, biology.In ceramic preparation method, blank forming is a key link.Conventional molding process (as isostatic pressing, injection molding, pressure filtration molding technology etc.) or can only shaping simple shape goods, or technological process reaches nearly hundred hours, expensive equipment must be coordinated simultaneously, and there is the shortcomings such as blank density is low, lack of homogeneity, intensity are low, firing deformation is large.Along with the development of industry, improve constantly the requirement of ceramic performance, conventional molding process can not meet the requirement of some industrial circles.
Summary of the invention
The present invention is intended to propose the aperture that produces in the process that a kind of addition by improving organic monomer and a large amount of gel moleculars of being formed discharge at pyrolytic decomposition and micropore, makes the method for the micro-porous ceramics of silicon nitride.
Technical program of the present invention lies in:
Gel casting forming prepares a method for micro-porous silicon nitride ceramic, adopts following steps:
Polyacrylamide is dissolved in deionized water, adds monomer, linking agent and dispersion agent after mechanical stirring 10min, forms premixed liquid; Then in this premixed liquid, add beta-silicon nitride powder and sintering aid, adjust ph is 11, and after ball milling 12h, obtained slurry, adds initiator degasification again, then injection molding after slurry vacuum stripping, at 65 DEG C of reaction 40min, slurry gelling is solidified, the demoulding; Finally dry under the condition of temperature 25 DEG C with humidity 98%; Based on base substrate after drying, carry out degreasing operation, sinter after degreasing it, insulation 1h, obtains ceramic sintered bodies.
Preferably, the concrete steps of described degreasing operation are: be increased to 200 DEG C from room temperature, and temperature rise rate is 60 DEG C/h, is increased to 550 DEG C from 200 DEG C, and temperature rise rate is 10 DEG C/h, and at 550 DEG C of insulation 8h.
Preferably, described sintering is with the ramp to 1730 DEG C of 10 DEG C/min in normal pressure nitrogen atmosphere.
Preferably, described sintering aid is the Al of massfraction 1%
2o
3and be the Y of 2% based on the massfraction of beta-silicon nitride powder
2o
3.
Preferably, described dry time condition be: temperature 25 DEG C and humidity 98%.
Technique effect of the present invention is:
The ceramic bending strength prepared by method provided by the invention is up to more than 137MPa, and void content is up to more than 50%, and hole central diameter is less than 1 μm, even aperture distribution, microtexture zero defect.
Embodiment
Gel casting forming prepares a method for micro-porous silicon nitride ceramic, adopts following steps:
Polyacrylamide is dissolved in deionized water, adds monomer, linking agent and dispersion agent after mechanical stirring 10min, forms premixed liquid; Then in this premixed liquid, add beta-silicon nitride powder and sintering aid, adjust ph is 11, and after ball milling 12h, obtained slurry, adds initiator degasification again, then injection molding after slurry vacuum stripping, at 65 DEG C of reaction 40min, slurry gelling is solidified, the demoulding; Finally dry under the condition of temperature 25 DEG C with humidity 98%; Based on base substrate after drying, carry out degreasing operation, sinter after degreasing it, insulation 1h, obtains ceramic sintered bodies.
Wherein, the concrete steps of degreasing operation are: be increased to 200 DEG C from room temperature, and temperature rise rate is 60 DEG C/h, is increased to 550 DEG C from 200 DEG C, and temperature rise rate is 10 DEG C/h, and at 550 DEG C of insulation 8h.Sintering is with the ramp to 1730 DEG C of 10 DEG C/min in normal pressure nitrogen atmosphere.
Preferably, described sintering aid is the Al of massfraction 1%
2o
3and be the Y of 2% based on the massfraction of beta-silicon nitride powder
2o
3.Condition time dry is: temperature 25 DEG C and humidity 98%.
Claims (5)
1. gel casting forming prepares a method for micro-porous silicon nitride ceramic, it is characterized in that: adopt following steps:
Polyacrylamide is dissolved in deionized water, adds monomer, linking agent and dispersion agent after mechanical stirring 10min, forms premixed liquid; Then in this premixed liquid, add beta-silicon nitride powder and sintering aid, adjust ph is 11, and after ball milling 12h, obtained slurry, adds initiator degasification again, then injection molding after slurry vacuum stripping, at 65 DEG C of reaction 40min, slurry gelling is solidified, the demoulding; Finally dry under the condition of temperature 25 DEG C with humidity 98%; Based on base substrate after drying, carry out degreasing operation, sinter after degreasing it, insulation 1h, obtains ceramic sintered bodies.
2. as claim 1 gel casting forming prepares the method for micro-porous silicon nitride ceramic, it is characterized in that: the concrete steps of described degreasing operation are: be increased to 200 DEG C from room temperature, temperature rise rate is 60 DEG C/h, 550 DEG C are increased to from 200 DEG C, temperature rise rate is 10 DEG C/h, and at 550 DEG C of insulation 8h.
3. as claim 1 gel casting forming prepares the method for micro-porous silicon nitride ceramic, it is characterized in that: described sintering is with the ramp to 1730 DEG C of 10 DEG C/min in normal pressure nitrogen atmosphere.
4., as claim 1 gel casting forming prepares the method for micro-porous silicon nitride ceramic, it is characterized in that: described sintering aid is the Al of massfraction 1%
2o
3and be the Y of 2% based on the massfraction of beta-silicon nitride powder
2o
3.
5., as claim 1 gel casting forming prepares the method for micro-porous silicon nitride ceramic, it is characterized in that: described dry time condition be: temperature 25 DEG C and humidity 98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510761777.4A CN105523773A (en) | 2015-11-11 | 2015-11-11 | Method for preparing micro-porous silicon nitride ceramic through gel casting |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510761777.4A CN105523773A (en) | 2015-11-11 | 2015-11-11 | Method for preparing micro-porous silicon nitride ceramic through gel casting |
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| CN105523773A true CN105523773A (en) | 2016-04-27 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187123A (en) * | 2016-06-30 | 2016-12-07 | 广东工业大学 | Aluminium oxide ceramics and preparation method thereof and plasma etch apparatus |
| CN107353015A (en) * | 2017-08-08 | 2017-11-17 | 中南大学 | A kind of porous composite ceramics preparation method of silicon carbide nitride silicon |
| CN108298992A (en) * | 2018-03-06 | 2018-07-20 | 济南大学 | A kind of method that environment-friendly type gel casting forming prepares silicon nitride ceramics biscuit |
| CN111635219A (en) * | 2019-03-01 | 2020-09-08 | 福建省德化福杰陶瓷有限公司 | Preparation method of silencing micropore artistic decorative ceramic tile |
-
2015
- 2015-11-11 CN CN201510761777.4A patent/CN105523773A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187123A (en) * | 2016-06-30 | 2016-12-07 | 广东工业大学 | Aluminium oxide ceramics and preparation method thereof and plasma etch apparatus |
| CN106187123B (en) * | 2016-06-30 | 2019-03-12 | 广东工业大学 | Aluminium oxide ceramics and preparation method thereof and plasma etch apparatus |
| CN107353015A (en) * | 2017-08-08 | 2017-11-17 | 中南大学 | A kind of porous composite ceramics preparation method of silicon carbide nitride silicon |
| CN107353015B (en) * | 2017-08-08 | 2020-03-10 | 中南大学 | Preparation method of silicon carbide-silicon nitride porous composite ceramic |
| CN108298992A (en) * | 2018-03-06 | 2018-07-20 | 济南大学 | A kind of method that environment-friendly type gel casting forming prepares silicon nitride ceramics biscuit |
| CN111635219A (en) * | 2019-03-01 | 2020-09-08 | 福建省德化福杰陶瓷有限公司 | Preparation method of silencing micropore artistic decorative ceramic tile |
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Application publication date: 20160427 |