CN105294111A - Gelcasting forming method of Si3N4 porous ceramic - Google Patents
Gelcasting forming method of Si3N4 porous ceramic Download PDFInfo
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- CN105294111A CN105294111A CN201510630894.7A CN201510630894A CN105294111A CN 105294111 A CN105294111 A CN 105294111A CN 201510630894 A CN201510630894 A CN 201510630894A CN 105294111 A CN105294111 A CN 105294111A
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Abstract
The invention relates to a gelcasting forming method of Si3N4 porous ceramic. Si3N4 micro powder, a sintering aid organic monomer and cross-linking agent are fully mixed and subjected to ball milling in deionized water, the obtained mixture generates crosslinking under a certain catalytic action after being injected into a mold, a three-dimensional reticular structure is formed so as to cause slurry to be subjected to in-situ curing forming, and a Si3N4 green body with a complex shape can be obtained. Through a method that the addition of the organic monomer is improved to decompose and generate small holes at a high temperature, a porous structure is formed. The Si3N4 porous ceramic prepared by the method has the advantages of high porosity, small aperture, evenly-distributed aperture and the like.
Description
Technical field
The invention belongs to field of inorganic materials, be related specifically to a kind of gel-casting method of porous SiN 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.
Adding pore-forming material and stirring foaming is the common method preparing porous ceramics, and the globule size of pore-forming material is often different, therefore causes pore-forming material can not be uniformly distributed in base substrate, makes even air hole distribution poor.And add tensio-active agent stir bubble, the aperture of polyurethane foam attached gel injection molding gained porous insert is comparatively large, so to stir the micro-porous ceramicss of making such as foamings, polyurethane foam attached gel injection molding all undesirable by adding the pore-forming materials such as carbon dust, starch, polyvinyl alcohol and tensio-active agent.
Summary of the invention
The present invention, by the aperture that produces in the process that improves the addition of organic monomer and a large amount of gel moleculars of being formed and discharge at pyrolytic decomposition and micropore, makes the micro-porous ceramics of silicon nitride.
The object of the invention to solve the technical problems realizes by the following technical solutions.The gel-casting method of a kind of porous SiN ceramic proposed according to the present invention, comprise following steps: by silicon nitride powder, sintering aid organic monomer and linking agent abundant mixing and ball milling in deionized water, occur crosslinked after injecting mould under katalysis, form tridimensional network thus make slip in-situ solidifying shaping, complex-shaped silicon nitride base substrate can be obtained, by improving organic monomer add-on, the method that pyrolytic decomposition produces aperture forms vesicular structure.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
The gel-casting method of aforesaid a kind of porous SiN ceramic, described silicon nitride powder is mainly α phase (>94%), and powder mean particle sizes is 0.3-0.4 μm; Described sintering aid is Al2O3 and Y2O3, and mean particle size is respectively 1-2 μm, 4-5 μm.
The gel-casting method of aforementioned a kind of porous SiN ceramic, described monomer is acrylamide, linking agent is methylene-bisacrylamide, and dispersion agent is ammonium polyacrylate, and initiator is ammonium persulphate.
Porous SiN ceramic prepared by the present invention has the advantages such as higher porosity, aperture are less, uniform pore diameter distribution.Preparation for porous SiN ceramic provides a kind of method that feasibility is high.
Embodiment
Below in conjunction with specific embodiment, book is described in detail to the present invention.
Embodiment 1
1. configure premixed liquid: be dissolved in deionized water by organic monomer, linking agent and dispersion agent, organic monomer add-on is 15% of deionized water quality, and the ratio of monomer and linking agent chooses 5: 1.
2. mixing and ball milling: above-mentioned premixed liquid and silicon nitride powder, sintering aid are put into ball mill fully mixing and ball milling, Al2O3 add-on is 1%, Y2O3 add-on of silicon nitride is 2% of silicon nitride, and Ball-milling Time is 5 hours, ratio of grinding media to material: 1: 1 ~ 3: 1.
3. vacuum stripping: add appropriate initiator A PS and catalyzer TEMED again, mix rear use vacuum mixer and be evacuated to 0.1Mpa, the degasification time is 10 minutes.
4. gel-casting: above-mentioned slip is injected ready mould, mould should use as impermeable metal, glass, plastics or waxed work, 40 DEG C of heating in air dry oven, in mould slip can gel solidification shaping;
7. the demoulding is dry: after slurry gel solidification, and after drying in 8 hours, gel base substrate is taken out in die sinking, is placed in air, at ambient temperature seasoning, is then placed in baking oven and dries further under 120 DEG C of conditions.
8. high temperature sintering: the base substrate after oven dry, 500 DEG C of insulations, makes polymkeric substance fully decompose, be more slowly warming up to 1700 DEG C-1750 DEG C insulation 1h sinter moldings.Porosity can be obtained more than 50%, the porous SiN ceramic that aperture is less than 1 μm.
Embodiment 2
1. configure premixed liquid: be dissolved in deionized water by organic monomer, linking agent and dispersion agent, organic monomer add-on is the 15-25% of deionized water quality, and the ratio of monomer and linking agent chooses 7: 1.
2. mixing and ball milling: above-mentioned premixed liquid and silicon nitride powder, sintering aid are put into ball mill fully mixing and ball milling, Al2O3 add-on is 1%, Y2O3 add-on of silicon nitride is 2% of silicon nitride, and Ball-milling Time is 7 hours, ratio of grinding media to material: 1: 1 ~ 3: 1.
3. vacuum stripping: add appropriate initiator A PS and catalyzer TEMED again, mix rear use vacuum mixer and be evacuated to 0.1Mpa, the degasification time is 20 minutes.
4. gel-casting: above-mentioned slip is injected ready mould, mould should use as impermeable metal, glass, plastics or waxed work, 50 DEG C of heating in air dry oven, in mould slip can gel solidification shaping;
7. the demoulding is dry: after slurry gel solidification, and after drying in 10 hours, gel base substrate is taken out in die sinking, is placed in air, at ambient temperature seasoning, is then placed in baking oven and dries further under 130 DEG C of conditions.
8. high temperature sintering: the base substrate after oven dry, 550 DEG C of insulations, makes polymkeric substance fully decompose, be more slowly warming up to 1700 DEG C-1750 DEG C insulation 1h sinter moldings.Porosity can be obtained more than 50%, the porous SiN ceramic that aperture is less than 1 μm.
Embodiment 3
1. configure premixed liquid: be dissolved in deionized water by organic monomer, linking agent and dispersion agent, organic monomer add-on is the 15-25% of deionized water quality, and the ratio of monomer and linking agent chooses 10: 1.
2. mixing and ball milling: above-mentioned premixed liquid and silicon nitride powder, sintering aid are put into ball mill fully mixing and ball milling, Al2O3 add-on is 1%, Y2O3 add-on of silicon nitride is 2% of silicon nitride, and Ball-milling Time is 10 hours, ratio of grinding media to material: 1: 1 ~ 3: 1.
3. vacuum stripping: add appropriate initiator A PS and catalyzer TEMED again, mix rear use vacuum mixer and be evacuated to 0.1Mpa, the degasification time is 30 minutes.
4. gel-casting: above-mentioned slip is injected ready mould, mould should use as impermeable metal, glass, plastics or waxed work, 60 DEG C of heating in air dry oven, in mould slip can gel solidification shaping;
7. the demoulding is dry: after slurry gel solidification, and after drying in 12 hours, gel base substrate is taken out in die sinking, is placed in air, at ambient temperature seasoning, is then placed in baking oven and dries further under 150 DEG C of conditions.
8. high temperature sintering: the base substrate after oven dry, 500-600 DEG C of insulation, makes polymkeric substance fully decompose, be more slowly warming up to 1700 DEG C-1750 DEG C insulation 1h sinter moldings.Porosity can be obtained more than 50%, the porous SiN ceramic that aperture is less than 1 μm.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (3)
1. the gel-casting method of a porous SiN ceramic, it is characterized in that, comprise following steps: by silicon nitride powder, sintering aid organic monomer and linking agent abundant mixing and ball milling in deionized water, occur crosslinked after injecting mould under katalysis, form tridimensional network thus make slip in-situ solidifying shaping, can obtain complex-shaped silicon nitride base substrate, by improving organic monomer add-on, the method that pyrolytic decomposition produces aperture forms vesicular structure.
2. the gel-casting method of a kind of porous SiN ceramic according to claim 1, it is characterized in that, described silicon nitride powder is mainly α phase (>94%), and powder mean particle sizes is 0.3-0.4 μm; Described sintering aid is Al2O3 and Y2O3, and mean particle size is respectively 1-2 μm, 4-5 μm.
3. the gel-casting method of a kind of porous SiN ceramic according to claim 1, it is characterized in that, described monomer is acrylamide, linking agent is methylene-bisacrylamide, and dispersion agent is ammonium polyacrylate, and initiator is ammonium persulphate.
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| CN201510630894.7A CN105294111A (en) | 2015-09-29 | 2015-09-29 | Gelcasting forming method of Si3N4 porous ceramic |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278348A (en) * | 2016-08-02 | 2017-01-04 | 宁波东联密封件有限公司 | The preparation method of pressureless sintering carborundum gel |
| CN106380204A (en) * | 2016-08-30 | 2017-02-08 | 宁波东联密封件有限公司 | Preparation method of silicon carbide composite material |
| CN107344865A (en) * | 2017-06-15 | 2017-11-14 | 上海极率科技有限公司 | The preparation method of heat transfer anisotropic ceramics material |
| 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 |
| CN111960838A (en) * | 2020-08-31 | 2020-11-20 | 武汉科技大学 | Silicon nitride framework reinforced quartz-based ceramic for photovoltaic silicon smelting and preparation method thereof |
| CN112811913A (en) * | 2021-03-11 | 2021-05-18 | 无锡辰海新材料科技有限公司 | Method for preparing silicon nitride ceramic biscuit by environment-friendly gel injection molding |
| CN112973286A (en) * | 2021-03-30 | 2021-06-18 | 烟台核晶陶瓷新材料有限公司 | Novel ceramic filter plate and manufacturing process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101503298A (en) * | 2009-03-13 | 2009-08-12 | 西安交通大学 | Method for preparing silicon nitride porous ceramic by gel injection moulding |
| CN103482981A (en) * | 2013-08-30 | 2014-01-01 | 航天特种材料及工艺技术研究所 | Preparation method of porous silicon nitride ceramic material |
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2015
- 2015-09-29 CN CN201510630894.7A patent/CN105294111A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503298A (en) * | 2009-03-13 | 2009-08-12 | 西安交通大学 | Method for preparing silicon nitride porous ceramic by gel injection moulding |
| CN103482981A (en) * | 2013-08-30 | 2014-01-01 | 航天特种材料及工艺技术研究所 | Preparation method of porous silicon nitride ceramic material |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278348A (en) * | 2016-08-02 | 2017-01-04 | 宁波东联密封件有限公司 | The preparation method of pressureless sintering carborundum gel |
| CN106380204A (en) * | 2016-08-30 | 2017-02-08 | 宁波东联密封件有限公司 | Preparation method of silicon carbide composite material |
| CN107344865A (en) * | 2017-06-15 | 2017-11-14 | 上海极率科技有限公司 | The preparation method of heat transfer anisotropic ceramics material |
| 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 |
| CN111960838A (en) * | 2020-08-31 | 2020-11-20 | 武汉科技大学 | Silicon nitride framework reinforced quartz-based ceramic for photovoltaic silicon smelting and preparation method thereof |
| CN111960838B (en) * | 2020-08-31 | 2022-01-14 | 武汉科技大学 | Silicon nitride framework reinforced quartz-based ceramic for photovoltaic silicon smelting and preparation method thereof |
| CN112811913A (en) * | 2021-03-11 | 2021-05-18 | 无锡辰海新材料科技有限公司 | Method for preparing silicon nitride ceramic biscuit by environment-friendly gel injection molding |
| CN112973286A (en) * | 2021-03-30 | 2021-06-18 | 烟台核晶陶瓷新材料有限公司 | Novel ceramic filter plate and manufacturing process thereof |
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Application publication date: 20160203 |