CN109320256A - A kind of silicon nitride-silicon carbide ceramic composite and preparation method thereof - Google Patents
A kind of silicon nitride-silicon carbide ceramic composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of silicon nitride-silicon carbide ceramic composites, also disclose the preparation method of the composite material, it include: (1) using beta-silicon nitride powder and silicon carbide powder as raw material, add sintering aid, deionized water is added, 60~90min of ball milling mixing obtains silicon nitride-silicon carbide slurry, wherein, the sintering aid includes 10~15% Al for accounting for beta-silicon nitride powder and silicon carbide powder raw material gross weight meter2O3With 5~8% Y2O3；(2) above-mentioned silicon nitride-silicon carbide slurry is filtered by vacuum, is dried under the conditions of 80~100 DEG C, is sieved, dry-pressing formed, and cold isostatic compaction under the conditions of 20~300MPa is carried out under the conditions of 1~10MPa, obtains silicon nitride-silicon carbide biscuit；(3) it will be put into sintering furnace after above-mentioned silicon nitride-silicon carbide biscuit, 1~3h is sintered under the conditions of 0.5~1.5MPa nitrogen atmosphere and 1250~1500 DEG C of temperature, and 1~2 hour is kept the temperature under the conditions of 1250~1500 DEG C, and it is cooling, obtain silicon nitride-silicon carbide ceramic composite.Preparation process of the present invention is simple, and ceramics bending strength and fracture toughness obtained are high.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of silicon nitride-silicon carbide ceramic composite and its system
Preparation Method.
Background technique
Silicon nitride and silicon carbide complex phase porous ceramics are due to good etc. with high tough, wear-resisting, corrosion-resistant and chemical stability
Advantage is all shown wide in fields such as high temperature air filtration, sensor, catalyst carrier, seperation film, heat insulators
Application prospect.
SiC powder, Si are used in patent ZL1019138783N4Powder and sintering aid and paraffinic base Multi-component binder are mixed
Uniform feeding is synthesized, feeding takes off through the resulting preform of injection moulding through solution-off, heat, after 1150~1200 DEG C of pre-sinterings,
It is normal pressure-sintered under 1800~1900 DEG C, Ar atmosphere to be placed in vacuum carbon tube furnace, has obtained the SiCp/Si of size complexity3N4Composite ceramic
Porcelain part material.Jian-Feng Yang et al. (Jian-Feng Yang, Tohro Sekino, Yong-Ho Choa, J Am
Ceram Soc84 (2001) 406-12) use α-Si3N4With SiC powder, sintering aid MgAlO is added4And ZrO2, pre- through 20MPa
The static pressure such as pressure and 200MPa are put into graphite resistor furnace 1800 DEG C of heat preservation 2-16h in the high pure nitrogen of 0.6Mpa and carry out atmosphere
Sintering, is then placed in 1800 DEG C of hot isostatic pressing furnaces and keeps the temperature 2h, apply the nitrogen pressure of 150MPa, finally obtained diverse microcosmic
The Si of the simple shape of structure and morphology3N4/ SiC composite ceramics, not only complex process, temperature high (1800 DEG C), reaction time are long
(4~18h).And when nitridation reaction, local temperature is excessively high, has been more than the fusing point of Si, so that Si is melted volatilization, reduces nitriding rate,
Although porosity improves, mechanical property is also reduced.
When above two reaction sintering technology complexity, consumption energy consumption, and it is difficult to control Si3N4The sky of/SiC complex phase porous ceramics
Gap distribution；And there is Si3N4/ SiC complex phase porous ceramic film material gap structure is uneven, orientation interconnectivity is poor, dead size molding
Difference, the technical problems such as bending strength is low.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of silicon nitride-silicon carbide ceramic composite and its preparation side
Method is able to solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of silicon nitride-silicon carbide ceramic composites and preparation method thereof, to overcome
Deficiency in the prior art.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of silicon nitride-silicon carbide ceramic composite, comprising the following steps:
(1) using beta-silicon nitride powder and silicon carbide powder as raw material, sintering aid is added, adds deionized water, ball milling is mixed
60~90min is closed, silicon nitride-silicon carbide slurry is obtained, wherein the sintering aid includes accounting for beta-silicon nitride powder and carborundum powder
10~15% Al of body raw material gross weight meter2O3With 5~8% Y2O3；
(2) above-mentioned silicon nitride-silicon carbide slurry is filtered by vacuum, is dried under the conditions of 80~100 DEG C, is sieved, 1~
Dry-pressing formed, and cold isostatic compaction under the conditions of 20~300MPa is carried out under the conditions of 10MPa, obtains silicon nitride-silicon carbide element
Base；
(3) it will be put into sintering furnace after above-mentioned silicon nitride-silicon carbide biscuit, in 0.5~1.5MPa nitrogen atmosphere and 1250
It is sintered 1~3h under the conditions of~1500 DEG C of temperature, and keeps the temperature 1~2 hour under the conditions of 1250~1500 DEG C, it is cooling, it obtains
Silicon nitride-silicon carbide ceramic composite.
Preferably, in step (1), the preparation method of the beta-silicon nitride powder includes: the alkali metal 1) using silicon halide as raw material
It for reducing agent, is weighed according to the mol ratio of reaction, reducing agent excessive 0~10% carries out reduction reaction, also in liquid ammonia medium
Former temperature is in -60 DEG C~20 DEG C ranges；2) it is purified by liquid phase, separating by-products obtain amorphous nano alpha-silicon nitride powders；3)
Through Overheating Treatment, it is converted into stable crystalline state nano-silicon nitride, i.e. Si3N4Powder.
Preferably, in step (1), the weight ratio of the beta-silicon nitride powder and silicon carbide powder is 1:1~3.
Preferably, in step 1), the silicon halide is selected from one of silicon chloride, silicon bromide, iodate silicon, the alkali metal
Selected from metallic sodium or metallic potassium.
It is multiple that technical solution of the present invention also provides a kind of silicon nitride-silicon carbide ceramics obtained according to above-mentioned preparation method
Condensation material.
Compared with the prior art, the advantages of the present invention are as follows: in the present invention, preparation process of the present invention is simple, by this hair
The bending strength and fracture toughness of silicon nitride-silicon carbide ceramic composite made from method in bright are high.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of silicon nitride-silicon carbide ceramic composite, comprising the following steps:
(1) using beta-silicon nitride powder and silicon carbide powder as raw material, sintering aid is added, adds deionized water, ball milling is mixed
60~90min is closed, silicon nitride-silicon carbide slurry is obtained, wherein the sintering aid includes accounting for beta-silicon nitride powder and carborundum powder
10~15% Al of body raw material gross weight meter2O3With 5~8% Y2O3；
(2) above-mentioned silicon nitride-silicon carbide slurry is filtered by vacuum, is dried under the conditions of 80~100 DEG C, is sieved, 1~
Dry-pressing formed, and cold isostatic compaction under the conditions of 20~300MPa is carried out under the conditions of 10MPa, obtains silicon nitride-silicon carbide element
Base；
(3) it will be put into sintering furnace after above-mentioned silicon nitride-silicon carbide biscuit, in 0.5~1.5MPa nitrogen atmosphere and 1250
It is sintered 1~3h under the conditions of~1500 DEG C of temperature, and keeps the temperature 1~2 hour under the conditions of 1250~1500 DEG C, it is cooling, it obtains
Silicon nitride-silicon carbide ceramic composite.
In above-mentioned steps (1), the weight ratio of the beta-silicon nitride powder and silicon carbide powder is 1:1~3, it is preferred that described
The weight ratio of beta-silicon nitride powder and silicon carbide powder is 1:1.
In above-mentioned steps (1), the preparation method of the beta-silicon nitride powder includes: 1) using silicon halide as raw material, and alkali metal is
Reducing agent is weighed according to the mol ratio of reaction, and reducing agent excessive 0~10% carries out reduction reaction in liquid ammonia medium, restores
Temperature is in -60 DEG C~20 DEG C ranges；2) it is purified by liquid phase, separating by-products obtain amorphous nano alpha-silicon nitride powders；3) it passes through
Overheating Treatment is converted into stable crystalline state nano-silicon nitride, i.e. Si3N4Powder.
Wherein, in step 1), the silicon halide is selected from one of silicon chloride, silicon bromide, iodate silicon, the alkali metal choosing
From metallic sodium or metallic potassium.
Embodiment
The preparation method of silicon nitride-silicon carbide ceramic composite, comprising the following steps:
(1) using silicon carbide powder and according to made from the above method, beta-silicon nitride powder is raw material, addition sintering aid, then plus
Enter deionized water, 60~90min of ball milling mixing obtains silicon nitride-silicon carbide slurry, wherein the beta-silicon nitride powder and carbonization
The weight ratio of silicon powder is 1:1, and the sintering aid includes accounting for beta-silicon nitride powder and silicon carbide powder raw material gross weight meter
12% Al2O3With 7.5% Y2O3；
(2) above-mentioned silicon nitride-silicon carbide slurry is filtered by vacuum, is dried under the conditions of 80 DEG C, is sieved, under the conditions of 5MPa into
Row is dry-pressing formed, and cold isostatic compaction under the conditions of 240MPa, obtains silicon nitride-silicon carbide biscuit；
(3) it will be put into sintering furnace after above-mentioned silicon nitride-silicon carbide biscuit, in 1MPa nitrogen atmosphere and 1400 DEG C of temperature strips
It is sintered 1.5h under part, and keeps the temperature 1~2 hour under the conditions of 1250 DEG C, it is cooling, obtain silicon nitride-silicon carbide Ceramic Composite
Material.
It is multiple that technical solution of the present invention also provides a kind of silicon nitride-silicon carbide ceramics obtained according to above-mentioned preparation method
Condensation material.It is strong using the progress bending resistance of three-point bending fracture method to silicon nitride-silicon carbide ceramic composite obtained in the present invention
Degree test, carries out fracture toughness test using single side notched beam three-point bending fracture method, mechanical property result: bending strength is
426MPa, fracture toughness 4.68MPam1/2。
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (5)
1. a kind of preparation method of silicon nitride-silicon carbide ceramic composite, which comprises the following steps:
(1) using beta-silicon nitride powder and silicon carbide powder as raw material, sintering aid is added, deionized water, ball milling mixing 60 are added
~90min obtains silicon nitride-silicon carbide slurry, wherein the sintering aid includes accounting for beta-silicon nitride powder and silicon carbide powder original
Expect 10~15% Al of total weight2O3With 5~8% Y2O3；
(2) above-mentioned silicon nitride-silicon carbide slurry is filtered by vacuum, is dried under the conditions of 80~100 DEG C, is sieved, in 1~10MPa item
Dry-pressing formed, and cold isostatic compaction under the conditions of 20~300MPa is carried out under part, obtains silicon nitride-silicon carbide biscuit；
(3) will be put into sintering furnace after above-mentioned silicon nitride-silicon carbide biscuit, 0.5~1.5MPa nitrogen atmosphere and 1250~
It is sintered 1~3h under the conditions of 1500 DEG C of temperature, and keeps the temperature 1~2 hour under the conditions of 1250~1500 DEG C, it is cooling, obtain nitrogen
SiClx-composite silicon carbide ceramic material.
2. the preparation method of silicon nitride-silicon carbide ceramic composite according to claim 1, which is characterized in that step
(1) in, the preparation method of the beta-silicon nitride powder includes: 1) using silicon halide as raw material, and alkali metal is reducing agent, according to reaction
Mol ratio weighs, and reducing agent excessive 0~10% carries out reduction reaction, reduction temperature is at -60 DEG C~20 DEG C in liquid ammonia medium
Range；2) it is purified by liquid phase, separating by-products obtain amorphous nano alpha-silicon nitride powders；3) it through Overheating Treatment, is converted into steady
Fixed crystalline state nano-silicon nitride, i.e. Si3N4Powder.
3. the preparation method of silicon nitride-silicon carbide ceramic composite according to claim 1, which is characterized in that step
(1) in, the weight ratio of the beta-silicon nitride powder and silicon carbide powder is 1:1~3.
4. the preparation method of silicon nitride-silicon carbide ceramic composite according to claim 2, which is characterized in that step
1) in, the silicon halide is selected from one of silicon chloride, silicon bromide, iodate silicon, and the alkali metal is selected from metallic sodium or metallic potassium.
5. a kind of silicon nitride-silicon carbide ceramic composite that preparation method according to claim 1 obtains.
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Cited By (6)
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| CN110483060A (en) * | 2019-08-19 | 2019-11-22 | 福建华清电子材料科技有限公司 | A kind of high heat conductivity silicon nitride ceramics and preparation method thereof |
| CN110877980A (en) * | 2019-11-13 | 2020-03-13 | 中国科学院上海硅酸盐研究所 | High-strength silicon carbide/silicon nitride composite ceramic and preparation method thereof |
| CN111170752A (en) * | 2020-01-17 | 2020-05-19 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of silicon carbide ceramic matrix composite and silicon carbide ceramic matrix composite |
| CN114133246A (en) * | 2021-12-01 | 2022-03-04 | 湖南湘瓷科艺有限公司 | Based on carbon-based and ceramic-based composites |
| CN115385685A (en) * | 2021-10-09 | 2022-11-25 | 江苏三条鱼新材料科技有限公司 | Processing technology for ceramic pressure chamber of hot chamber die casting machine |
| CN116477957A (en) * | 2023-05-05 | 2023-07-25 | 湖南泰鑫瓷业有限公司 | Heat-resistant ceramic cutter and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110483060A (en) * | 2019-08-19 | 2019-11-22 | 福建华清电子材料科技有限公司 | A kind of high heat conductivity silicon nitride ceramics and preparation method thereof |
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| CN110877980A (en) * | 2019-11-13 | 2020-03-13 | 中国科学院上海硅酸盐研究所 | High-strength silicon carbide/silicon nitride composite ceramic and preparation method thereof |
| CN111170752A (en) * | 2020-01-17 | 2020-05-19 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of silicon carbide ceramic matrix composite and silicon carbide ceramic matrix composite |
| CN115385685A (en) * | 2021-10-09 | 2022-11-25 | 江苏三条鱼新材料科技有限公司 | Processing technology for ceramic pressure chamber of hot chamber die casting machine |
| CN114133246A (en) * | 2021-12-01 | 2022-03-04 | 湖南湘瓷科艺有限公司 | Based on carbon-based and ceramic-based composites |
| CN116477957A (en) * | 2023-05-05 | 2023-07-25 | 湖南泰鑫瓷业有限公司 | Heat-resistant ceramic cutter and preparation method and application thereof |
| CN116477957B (en) * | 2023-05-05 | 2024-03-12 | 湖南泰鑫瓷业有限公司 | Heat-resistant ceramic cutter and preparation method and application thereof |
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Application publication date: 20190212 |