CN112266266A - Porous silicon nitride ceramic and preparation method thereof - Google Patents
Porous silicon nitride ceramic and preparation method thereof Download PDFInfo
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- CN112266266A CN112266266A CN202011220473.4A CN202011220473A CN112266266A CN 112266266 A CN112266266 A CN 112266266A CN 202011220473 A CN202011220473 A CN 202011220473A CN 112266266 A CN112266266 A CN 112266266A
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Abstract
The invention discloses a porous silicon nitride ceramic and a preparation method thereof, wherein the porous silicon nitride ceramic is prepared from the following raw materials in parts by weight: 2-4 parts of silicon nitride powder, 3-9 parts of glycerol, 4-6 parts of sintering aid, 5-9 parts of binder, 6-8 parts of polystyrene, 3-7 parts of polyvinyl butyral, 2-4 parts of alumina, 3-6 parts of pore-forming agent, 3-5 parts of melamine, 4-8 parts of dispersant, 3-7 parts of formaldehyde, 4-8 parts of defoamer and 5-9 parts of ethyl orthosilicate, in the preparation process, the shrinkage rates of materials are close to the same through the arrangement of the glycerol and the polyvinyl butyral, so that the condition of cracks of the ceramic is prevented, the quality of the ceramic is improved, and when the ceramic material is mixed, the fusion effect among the materials is improved through the dispersant, thereby improving the sintering effect of the ceramic.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to porous silicon nitride ceramic and a preparation method thereof.
Background
Ceramics are a generic term for pottery and porcelain. The traditional ceramics are also called common ceramics, which are products fired by using natural silicate such as clay and the like as main raw materials, and the modern ceramics are also called novel ceramics, fine ceramics or special ceramics. It is usually made from non-silicate chemical raw materials or synthetic raw materials, such as oxides (alumina, zirconia, titania, etc.) and non-oxides (silicon nitride, boron carbide, etc.). The silicon nitride material has good thermal, electrical and mechanical properties. The porous silicon nitride ceramic has the characteristics of high temperature resistance, corrosion resistance, high strength, high wave transmittance and the like, and is the key point of the research of a new-generation antenna housing material. The porous silicon nitride ceramic material has excellent comprehensive properties of high specific strength, high temperature resistance, oxidation resistance, wear resistance, thermal shock resistance and the like, and also has excellent dielectric properties of relatively low density, low dielectric constant, dielectric loss and the like, and can be widely applied to important fields of machinery, chemical engineering, ocean engineering, aerospace and the like because the excellent properties of the silicon nitride ceramic and the porous ceramic can be fully exerted.
In the production process of the existing porous silicon nitride ceramic, due to different shrinkage rates, cracks are easy to appear, the quality of the ceramic is reduced, and meanwhile, when the ceramic material is mixed, the fusion effect between materials is poor, so that the sintering effect of the ceramic is influenced.
Disclosure of Invention
The present invention is directed to a porous silicon nitride ceramic and a method for preparing the same, which solves the above problems of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: the porous silicon nitride ceramic is prepared from the following raw materials in parts by weight: 2-4 parts of silicon nitride powder, 3-9 parts of glycerol, 4-6 parts of sintering aid, 5-9 parts of binder, 6-8 parts of polystyrene, 3-7 parts of polyvinyl butyral, 2-4 parts of aluminum oxide, 3-6 parts of pore-forming agent, 3-5 parts of melamine, 4-8 parts of dispersing agent, 3-7 parts of formaldehyde, 4-8 parts of defoaming agent and 5-9 parts of ethyl orthosilicate.
As further preferable in the present technical solution: the sintering aid is prepared from the following raw materials in parts by weight: 3-6 parts of yttrium oxide and 2-6 parts of water.
As further preferable in the present technical solution: the adhesive is prepared from the following raw materials in parts by weight: 4-8 parts of methyl cellulose and 2-6 parts of water.
As further preferable in the present technical solution: the pore-forming agent is prepared from the following raw materials in parts by weight: 3-6 parts of wood dust, 3-9 parts of adhesion promoter and 2-6 parts of water.
As further preferable in the present technical solution: the dispersing agent is prepared from the following raw materials in parts by weight: 2-6 parts of triethyl hexyl phosphoric acid, 3-5 parts of sodium dodecyl sulfate, 2-4 parts of methyl amyl alcohol, 3-6 parts of cellulose derivative, 5-7 parts of polyacrylamide and 5-7 parts of fatty acid polyglycol ester.
As further preferable in the present technical solution: the defoaming agent is prepared from the following raw materials in parts by weight: 4-6 parts of active ingredients, 5-7 parts of emulsifier and 5-9 parts of emulsification aid.
A preparation method of porous silicon nitride ceramics comprises the following steps:
s1, proportioning raw materials for preparing the porous silicon nitride ceramic for later use;
s2, adding silicon nitride powder, glycerin, a sintering aid, a binder, polystyrene, polyvinyl butyral, alumina, a pore-forming agent, melamine, a dispersing agent, formaldehyde, a defoaming agent and ethyl orthosilicate for preparing the porous silicon nitride ceramic into stirring equipment, wherein the stirring time is 40-60min, the rotating speed is 300-500r/min, and the temperature is 50-70 ℃;
s3, adding the material obtained in the step S2 into forming equipment for forming;
s4, sintering the ceramic blank formed in the S3 in sintering equipment, and meanwhile, adding a protective atmosphere of nitrogen, wherein the sintering time is 60-80min and the temperature is 600-800 ℃;
and S5, finally, sterilizing the ceramic product by a sterilizing device.
As further preferable in the present technical solution: in S5, the sterilizing time by the sterilizing equipment is 20-40 min.
Compared with the prior art, the invention has the beneficial effects that: in the preparation process, the shrinkage rates of the materials are nearly the same through the arrangement of the glycerol and the polyvinyl butyral, so that the condition of cracks of the ceramic is prevented, the quality of the ceramic is improved, and the blending effect of the materials is improved through the dispersant when the ceramic material is mixed, so that the sintering effect of the ceramic is improved.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1, the present invention provides a technical solution: the porous silicon nitride ceramic is prepared from the following raw materials in parts by weight: 2 parts of silicon nitride powder, 3 parts of glycerol, 4 parts of sintering aid, 5 parts of binder, 6 parts of polystyrene, 3 parts of polyvinyl butyral, 2 parts of alumina, 3 parts of pore-forming agent, 3 parts of melamine, 4 parts of dispersing agent, 3 parts of formaldehyde, 4 parts of defoaming agent and 5 parts of ethyl orthosilicate.
In this embodiment, specifically: the sintering aid is prepared from the following raw materials in parts by weight: 3 parts of yttrium oxide and 2 parts of water; by setting the sintering agent, reasonable sintered mineral composition and mineral phase structure are obtained by utilizing catalytic technology to strengthen sintering.
On the basis of the scheme: the adhesive is prepared from the following raw materials in parts by weight: 4 parts by weight of methyl cellulose and 2 parts by weight of water; increasing the viscosity between the materials.
Further: the pore-forming agent is prepared from the following raw materials in parts by weight: 3 parts of wood dust, 3 parts of adhesion promoter and 2 parts of water; the pores of the present invention are increased, making the present invention more porous.
As a still further scheme of the invention: the dispersing agent is prepared from the following raw materials in parts by weight: 2 parts by weight of triethylhexyl phosphoric acid, 3 parts by weight of sodium dodecyl sulfate, 2 parts by weight of methylpentanol, 3 parts by weight of cellulose derivative, 5 parts by weight of polyacrylamide and 5 parts by weight of fatty acid polyglycol ester; through the arrangement of the dispersing agent, the blending effect between the materials is better.
On the basis of the scheme: the defoaming agent is prepared from the following raw materials in parts by weight: 4 parts of active ingredients, 5 parts of emulsifying agents and 5 parts of emulsifying aids; through the setting of defoaming agent, eliminate the bubble that produces when stirring between the material.
A preparation method of porous silicon nitride ceramics comprises the following steps:
s1, proportioning raw materials for preparing the porous silicon nitride ceramic for later use;
s2, adding silicon nitride powder, glycerin, a sintering aid, a binder, polystyrene, polyvinyl butyral, alumina, a pore-forming agent, melamine, a dispersing agent, formaldehyde, a defoaming agent and tetraethoxysilane for preparing the porous silicon nitride ceramic into stirring equipment, wherein the stirring time is 40min, the rotating speed is 300r/min, and the temperature is 50 ℃;
s3, adding the material obtained in the step S2 into forming equipment for forming;
s4, placing the ceramic blank formed in the step S3 into sintering equipment for sintering, and meanwhile, adding a protective atmosphere of nitrogen, wherein the sintering time is 60min and the temperature is 600 ℃;
and S5, finally, sterilizing the ceramic product by a sterilizing device.
Further: in S5, the sterilization time by the sterilization apparatus is 20 min; eliminating residual bacteria in the production process of the invention.
Example two
Referring to fig. 1, the present invention provides a technical solution: the porous silicon nitride ceramic is prepared from the following raw materials in parts by weight: 3 parts of silicon nitride powder, 6 parts of glycerol, 5 parts of sintering aid, 7 parts of binder, 7 parts of polystyrene, 5 parts of polyvinyl butyral, 3 parts of alumina, 4 parts of pore-forming agent, 4 parts of melamine, 6 parts of dispersing agent, 5 parts of formaldehyde, 6 parts of defoaming agent and 7 parts of ethyl orthosilicate.
In this embodiment, specifically: the sintering aid is prepared from the following raw materials in parts by weight: 4 parts by weight of yttrium oxide and 4 parts by weight of water.
On the basis of the scheme: the adhesive is prepared from the following raw materials in parts by weight: 6 parts by weight of methylcellulose and 4 parts by weight of water.
Further: the pore-forming agent is prepared from the following raw materials in parts by weight: 5 parts of sawdust powder, 6 parts of adhesion promoter and 4 parts of water.
As a still further scheme of the invention: the dispersing agent is prepared from the following raw materials in parts by weight: 4 parts by weight of triethylhexyl phosphoric acid, 4 parts by weight of sodium dodecyl sulfate, 3 parts by weight of methylpentanol, 4 parts by weight of cellulose derivative, 6 parts by weight of polyacrylamide and 6 parts by weight of fatty acid polyglycol ester.
On the basis of the scheme: the defoaming agent is prepared from the following raw materials in parts by weight: 5 parts of active ingredients, 6 parts of emulsifying agents and 7 parts of emulsifying aids.
A preparation method of porous silicon nitride ceramics comprises the following steps:
s1, proportioning raw materials for preparing the porous silicon nitride ceramic for later use;
s2, adding silicon nitride powder, glycerin, a sintering aid, a binder, polystyrene, polyvinyl butyral, alumina, a pore-forming agent, melamine, a dispersing agent, formaldehyde, a defoaming agent and ethyl orthosilicate which are used for preparing the porous silicon nitride ceramic into stirring equipment, wherein the stirring time is 50min, the rotating speed is 400r/min, and the temperature is 60 ℃;
s3, adding the material obtained in the step S2 into forming equipment for forming;
s4, placing the ceramic blank formed in the step S3 into sintering equipment for sintering, and meanwhile, adding a protective atmosphere of nitrogen, wherein the sintering time is 70min and the temperature is 700 ℃;
and S5, finally, sterilizing the ceramic product by a sterilizing device.
Further: in S5, the sterilization time by the sterilization apparatus was 30 min.
EXAMPLE III
Referring to fig. 1, the present invention provides a technical solution: the porous silicon nitride ceramic is prepared from the following raw materials in parts by weight: 4 parts of silicon nitride powder, 9 parts of glycerol, 6 parts of sintering aid, 9 parts of binder, 8 parts of polystyrene, 7 parts of polyvinyl butyral, 4 parts of alumina, 6 parts of pore-forming agent, 5 parts of melamine, 8 parts of dispersing agent, 7 parts of formaldehyde, 8 parts of defoaming agent and 9 parts of ethyl orthosilicate.
In this embodiment, specifically: the sintering aid is prepared from the following raw materials in parts by weight: 6 parts by weight of yttrium oxide and 6 parts by weight of water.
On the basis of the scheme: the adhesive is prepared from the following raw materials in parts by weight: 8 parts by weight of methylcellulose and 6 parts by weight of water.
Further: the pore-forming agent is prepared from the following raw materials in parts by weight: 6 parts of wood dust, 9 parts of adhesion promoter and 6 parts of water.
As a still further scheme of the invention: the dispersing agent is prepared from the following raw materials in parts by weight: 6 parts of triethylhexyl phosphoric acid, 5 parts of sodium dodecyl sulfate, 4 parts of methyl amyl alcohol, 6 parts of cellulose derivative, 7 parts of polyacrylamide and 7 parts of fatty acid polyglycol ester.
On the basis of the scheme: the defoaming agent is prepared from the following raw materials in parts by weight: 6 parts of active ingredients, 7 parts of emulsifying agents and 9 parts of emulsifying aids.
A preparation method of porous silicon nitride ceramics comprises the following steps:
s1, proportioning raw materials for preparing the porous silicon nitride ceramic for later use;
s2, adding silicon nitride powder, glycerin, a sintering aid, a binder, polystyrene, polyvinyl butyral, alumina, a pore-forming agent, melamine, a dispersing agent, formaldehyde, a defoaming agent and ethyl orthosilicate which are used for preparing the porous silicon nitride ceramic into stirring equipment, wherein the stirring time is 60min, the rotating speed is 500r/min, and the temperature is 70 ℃;
s3, adding the material obtained in the step S2 into forming equipment for forming;
s4, placing the ceramic blank formed in the S3 into sintering equipment for sintering, and meanwhile, adding a protective atmosphere of nitrogen, wherein the sintering time is 80min and the temperature is 800 ℃;
and S5, finally, sterilizing the ceramic product by a sterilizing device.
Further: in S5, the sterilization time by the sterilization apparatus was 40 min.
When the ceramic material is used, the shrinkage rates of the materials are close to the same through the arrangement of the glycerol and the polyvinyl butyral in the preparation process, so that the cracking of the ceramic is prevented, the quality of the ceramic is improved, and the fusion effect of the materials is improved through the dispersing agent when the ceramic material is mixed, so that the sintering effect of the ceramic is improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A porous silicon nitride ceramic, characterized by: the composite material is prepared from the following raw materials in parts by weight: 2-4 parts of silicon nitride powder, 3-9 parts of glycerol, 4-6 parts of sintering aid, 5-9 parts of binder, 6-8 parts of polystyrene, 3-7 parts of polyvinyl butyral, 2-4 parts of aluminum oxide, 3-6 parts of pore-forming agent, 3-5 parts of melamine, 4-8 parts of dispersing agent, 3-7 parts of formaldehyde, 4-8 parts of defoaming agent and 5-9 parts of ethyl orthosilicate.
2. The porous silicon nitride ceramic of claim 1, wherein: the sintering aid is prepared from the following raw materials in parts by weight: 3-6 parts of yttrium oxide and 2-6 parts of water.
3. The porous silicon nitride ceramic of claim 1, wherein: the adhesive is prepared from the following raw materials in parts by weight: 4-8 parts of methyl cellulose and 2-6 parts of water.
4. The porous silicon nitride ceramic of claim 1, wherein: the pore-forming agent is prepared from the following raw materials in parts by weight: 3-6 parts of wood dust, 3-9 parts of adhesion promoter and 2-6 parts of water.
5. The porous silicon nitride ceramic of claim 1, wherein: the dispersing agent is prepared from the following raw materials in parts by weight: 2-6 parts of triethyl hexyl phosphoric acid, 3-5 parts of sodium dodecyl sulfate, 2-4 parts of methyl amyl alcohol, 3-6 parts of cellulose derivative, 5-7 parts of polyacrylamide and 5-7 parts of fatty acid polyglycol ester.
6. The porous silicon nitride ceramic of claim 1, wherein: the defoaming agent is prepared from the following raw materials in parts by weight: 4-6 parts of active ingredients, 5-7 parts of emulsifier and 5-9 parts of emulsification aid.
7. A preparation method of porous silicon nitride ceramics is characterized by comprising the following steps: the method comprises the following steps:
s1, proportioning raw materials for preparing the porous silicon nitride ceramic for later use;
s2, adding silicon nitride powder, glycerin, a sintering aid, a binder, polystyrene, polyvinyl butyral, alumina, a pore-forming agent, melamine, a dispersing agent, formaldehyde, a defoaming agent and ethyl orthosilicate for preparing the porous silicon nitride ceramic into stirring equipment, wherein the stirring time is 40-60min, the rotating speed is 300-500r/min, and the temperature is 50-70 ℃;
s3, adding the material obtained in the step S2 into forming equipment for forming;
s4, sintering the ceramic blank formed in the S3 in sintering equipment, and meanwhile, adding a protective atmosphere of nitrogen, wherein the sintering time is 60-80min and the temperature is 600-800 ℃;
and S5, finally, sterilizing the ceramic product by a sterilizing device.
8. The method according to claim 7, wherein the step of preparing the porous silicon nitride ceramic comprises: in S5, the sterilizing time by the sterilizing equipment is 20-40 min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962545A (en) * | 2006-11-28 | 2007-05-16 | 武汉理工大学 | Silicon nitride non-aqueous tape-casting slurry and its preparation method |
| CN101597177A (en) * | 2009-07-10 | 2009-12-09 | 清华大学 | A kind of preparation method of highly oriented tube-shaped through hole porous ceramics |
| CN103819196A (en) * | 2013-12-30 | 2014-05-28 | 莱鼎电子材料科技有限公司 | Modified aluminum nitride ceramic substrate and production method thereof |
| CN106823844A (en) * | 2017-01-23 | 2017-06-13 | 广东风华高新科技股份有限公司 | Porous membrane and preparation method thereof |
| CN106938935A (en) * | 2017-04-26 | 2017-07-11 | 南通博泰美术图案设计有限公司 | Modified aluminium nitride ceramic substrate and its production method |
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- 2020-11-05 CN CN202011220473.4A patent/CN112266266A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962545A (en) * | 2006-11-28 | 2007-05-16 | 武汉理工大学 | Silicon nitride non-aqueous tape-casting slurry and its preparation method |
| CN101597177A (en) * | 2009-07-10 | 2009-12-09 | 清华大学 | A kind of preparation method of highly oriented tube-shaped through hole porous ceramics |
| CN103819196A (en) * | 2013-12-30 | 2014-05-28 | 莱鼎电子材料科技有限公司 | Modified aluminum nitride ceramic substrate and production method thereof |
| CN106823844A (en) * | 2017-01-23 | 2017-06-13 | 广东风华高新科技股份有限公司 | Porous membrane and preparation method thereof |
| CN106938935A (en) * | 2017-04-26 | 2017-07-11 | 南通博泰美术图案设计有限公司 | Modified aluminium nitride ceramic substrate and its production method |
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