CN104119094B - Ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof - Google Patents
Ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof Download PDFInfo
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- CN104119094B CN104119094B CN201410391803.4A CN201410391803A CN104119094B CN 104119094 B CN104119094 B CN 104119094B CN 201410391803 A CN201410391803 A CN 201410391803A CN 104119094 B CN104119094 B CN 104119094B
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Abstract
Ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof, the ceramic base composition board of SiC whisker reinforcement comprises inorganic ceramic powder base material, chemical vapor infiltration (CVI)-SiC whisker, SiC whisker is embedded in ceramic base material, and combine closely with ceramic base material, inorganic ceramic powder base material volume fraction is 60% ~ 80%, and chemical vapor infiltration (CVI)-SiC whisker is 20% ~ 40%.Inorganic ceramic powder base material is silicon carbide, silicon nitride, boron nitride, norbide, and ceramic powder particle is of a size of 10 ~ 100um.Gel casting is adopted to prepare ceramic performs, in conjunction with chemical vapor infiltration (CVI) at precast body growth inside SiC whisker, densification ceramic performs.Gel casting is in conjunction with the ceramic base composition board of CVI legal system for SiC whisker reinforcement, and goods fracture toughness property and flexural strength improve, and work reliability is high.
Description
Technical field
The present invention relates to ceramic base composition board and preparation method thereof, particularly relate to ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof.
Background technology
Along with developing rapidly of science and technology, each industrial sectors such as machinery, electronics, aerospace, the energy propose higher requirement to the performance of material, existing metal or macromolecular material are often difficult to be competent at, and the stupalith therefore with excellent properties such as high rigidity, wear-resistant, corrosion-resistant, thermo-chemical stabilities receives publicity day by day.Meanwhile, the fragility of stupalith is large, and the weakness that toughness is low also becomes the focus of various countries' research.
Silicon carbide whisker (SiC
w) to be a kind of diameter be nano level is to the micron-sized single crystal fibre with height-oriented property, crystalline structure and diamond similar, in crystal, impurity atom is few, without grain boundary, crystal structure defects is few, crystallization phases uniform component, has high-melting-point (> 2700 DEG C), low density ((3.21g/cm
3), (tensile strength is 2100kg/cm to high strength
2), (Young's modulus is 4.9 × 104kg/cm to high elastic coefficient
2), low-thermal-expansion rate and wear-resisting, corrosion-resistant, the characteristic such as oxidation-resistance property is strong, have the good reputation of " king of whisker ".Silicon carbide whisker has synthesized the crystal whisker products that in whisker, hardness is the highest, Young's modulus is maximum, tensile strength is maximum, heat resisting temperature is the highest.The stupalith utilizing it larger to fragility carries out toughness reinforcing, improves the performance of stupalith, and being widely applied preparing in high performance composite, is also a kind of strongthener for studying more in toughening ceramic based composites.
The method of current production SiC whisker mainly contains solid material method and gas-phase reaction method.Solid material method utilizes carrier gas by carbon containing and siliceous solid material, forms SiC whisker in the space separated with reaction material.Solid material method is both economical, be applicable to suitability for industrialized production, but it is more difficult to prepare highly purified SiC whisker.Gas-phase reaction method reacts with carbonaceous gas and silicon-containing gas or decomposes the organic gas of a kind of carbon containing, silicon compound, synthesis SiC whisker, it is the most general that wherein chemical vapour deposition (CVD) and chemical vapor infiltration (CVI) technology are applied.The method has and can control to generate the silicon carbide whisker of different crystal forms, and gained silicon carbide whisker purity is higher, and technique is simple, and reaction process does not have corrodibility and the larger intermediate product of toxicity, and conversion unit is simple, convenient operation.
Application number is that the Chinese patent of 201110122040.X discloses SiC ceramic based composites of a kind of SiC whisker strengthening and preparation method thereof, matrix material is prepared by the reaction of Si or Si alloy infiltration by prefabricated component, and described prefabricated component is obtained by the raw material compression molding comprising SiC Whiskers from Rice Hulls product.This composite process preparation technology is simple, and infiltration temperature of reaction is low, and without the need to impressed pressure, prefabricated component can be made into complicated shape, can be used for preparing complex shaped components.
Application number be 201210088399.4 Chinese patent disclose the preparation technology of the toughness reinforcing zirconium diboride ceramics of a kind of silicon carbide whisker.Adopt sol-gel method at ZrB
2particle surface parcel SiO
2, add activated carbon after drying, grinding and fully mix, compound heating under the protection of flowing argon gas atmosphere, utilizes SiO
2carbothermic reduction reaction between-C is at ZrB
2surface in situ generates SiC
w, obtain ZrB
2-SiC
wpowder, then sintering prepares the toughness reinforcing zirconium diboride ceramic material of silicon carbide whisker.Solve SiC
wbe uniformly dispersed sex chromosome mosaicism in the substrate, improves the structure of material, improves the performance of material.
The silicon carbide whisker obtained in the preparation method of above-mentioned two kinds of matrix materials and reaction residue separation difficulty, foreign matter content is high, and particularly sepn process can reduce the quality of silicon carbide whisker, have impact on the enhancement of silicon carbide whisker to base material.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof is provided, it is characterized in that the ceramic base composition board of described SiC whisker reinforcement comprises inorganic ceramic powder base material, chemical vapor infiltration (CVI)-SiC whisker, SiC whisker is embedded in ceramic base material, and combine closely with ceramic base material, ceramic matric composite can be discoideus, square tabular etc.The method of gel casting is adopted to prepare ceramic performs.Inorganic ceramic powder base material volume fraction is 60% ~ 80%, and chemical vapor infiltration (CVI)-SiC whisker is 20% ~ 40%.Described inorganic ceramic powder base material can be silicon carbide, silicon nitride, boron nitride, norbide, and ceramic powder particle is of a size of 10 ~ 100um.
The present invention aims to provide a kind of preparation method of ceramic base composition board of SiC whisker reinforcement, it is characterized in that, comprises following sequential steps:
(1) adding monomeric acrylamide and linking agent methylene-bisacrylamide in aqueous, to form concentration be the premixed liquid of 10% ~ 20%;
(2) in the inorganic ceramic powder that proportioning is good, add premixed liquid and dispersants ammonium polyacrylate by 55% ~ 60% solid volume component requirement, regulate PH to 9 ~ 11, ball milling mixing 10 ~ 20h, makes slurry;
(3) add initiator ammonium persulfate after slurry exhaust, fully stir and inject die cavity after removing bubble, adding catalyzer Tetramethyl Ethylene Diamine, gelation 30 ~ 60min, place after the demoulding and steadily locates;
(4) above-mentioned base substrate is put into baking oven, temperature is 60 ~ 80 DEG C, drying time 8 ~ 12h;
(5), after drying, at 400 ~ 700 DEG C of removing forming agents that come unstuck, obtain precast body, then surface working, precision reaches sealing material level;
(6) above-mentioned precast body is put into Reaktionsofen, under vacuum atmosphere, be warming up to temperature of reaction, pass into certain trichloromethyl silane, hydrogen is as carrier gas, argon gas is as diluent gas, and temperature of reaction is 1000 ~ 1200 DEG C, and Trichloromonosilane flow is 30 ~ 50sccm, hydrogen flowing quantity is 200 ~ 300sccm, argon flow amount is 200 ~ 300sccm, controls reaction conditions, chemical vapor infiltration silicon carbide whisker, precast body densification, penetration time is 200 ~ 300h;
(7) complete densification post-treatment to original surface accuracy, finally obtain the ceramic base composition board of SiC whisker reinforcement.
The advantage that the present invention has: 1, precast body is prepared in gel casting, and blank strength is high, and porous nickel degree is good, is beneficial to perhaps chemical vapor infiltration SiC
w; 2, chemical vapor infiltration prepares SiC
wbe uniformly dispersed at intrinsic silicon, and combine closely, reinforced effects is better; 3, goods toughness improves, and fracture toughness property and flexural strength improve, and work reliability is high.
Accompanying drawing explanation
Fig. 1 is the sectional view of the ceramic base composition board of discoideus SiC whisker reinforcement.
10 is inorganic ceramic powder base material; 20 is chemical vapor infiltration (CVI)-SiC whisker.
Embodiment
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims and limited.
Embodiment 1
(1) adding monomeric acrylamide and linking agent methylene-bisacrylamide in aqueous, to form concentration be the premixed liquid of 15%;
(2) in the inorganic ceramic powder that proportioning is good, add premixed liquid and dispersants ammonium polyacrylate by 55% solid volume component requirement, regulate PH to 11, ball milling mixing 15h, makes slurry;
(3) add initiator ammonium persulfate after slurry exhaust, fully stir and inject die cavity after removing bubble, adding catalyzer Tetramethyl Ethylene Diamine, gelation 45min, place after the demoulding and steadily locates;
(4) above-mentioned base substrate is put into baking oven, temperature is 70 DEG C, drying time 12h;
(5), after drying, at 600 DEG C of removing forming agents that come unstuck, obtain precast body, then surface working, precision reaches sealing material level;
(6) above-mentioned precast body is put into Reaktionsofen, under vacuum atmosphere, be warming up to temperature of reaction, pass into certain trichloromethyl silane, hydrogen is as carrier gas, argon gas is as diluent gas, and temperature of reaction is 1100 DEG C, and Trichloromonosilane flow is 30sccm, hydrogen flowing quantity is 300sccm, argon flow amount is 300sccm, controls reaction conditions, chemical vapor infiltration silicon carbide whisker, precast body densification, penetration time is 300h;
(7) complete densification post-treatment to original surface accuracy, finally obtain the ceramic base composition board of SiC whisker reinforcement.
Embodiment 2
(1) adding monomeric acrylamide and linking agent methylene-bisacrylamide in aqueous, to form concentration be the premixed liquid of 20%;
(2) in the inorganic ceramic powder that proportioning is good, add premixed liquid and dispersants ammonium polyacrylate by 60% solid volume component requirement, regulate PH to 10, ball milling mixing 20h, makes slurry;
(3) add initiator ammonium persulfate after slurry exhaust, fully stir and inject die cavity after removing bubble, adding catalyzer Tetramethyl Ethylene Diamine, gelation 60min, place after the demoulding and steadily locates;
(4) above-mentioned base substrate is put into baking oven, temperature is 80 DEG C, drying time 10h;
(5), after drying, at 700 DEG C of removing forming agents that come unstuck, obtain precast body, then surface working, precision reaches sealing material level;
(6) above-mentioned precast body is put into Reaktionsofen, under vacuum atmosphere, be warming up to temperature of reaction, pass into certain trichloromethyl silane, hydrogen is as carrier gas, argon gas is as diluent gas, and temperature of reaction is 1000 DEG C, and Trichloromonosilane flow is 50sccm, hydrogen flowing quantity is 300sccm, argon flow amount is 300sccm, controls reaction conditions, chemical vapor infiltration silicon carbide whisker, precast body densification, penetration time is 250h;
(7) complete densification post-treatment to original surface accuracy, finally obtain the ceramic base composition board of SiC whisker reinforcement.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited thereto, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content not departing from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (1)
1. a preparation method for the ceramic base composition board of SiC whisker reinforcement, is characterized in that comprising following sequential steps:
(1) add in water solvent monomeric acrylamide and linking agent methylene-bisacrylamide formed concentration 10% ~ 20% premixed liquid;
(2) in the inorganic ceramic powder that proportioning is good, add premixed liquid and dispersants ammonium polyacrylate by 55% ~ 60% total solid volume component requirement, regulate PH to 9 ~ 11, ball milling mixing 10 ~ 20h, makes slurry;
(3) add initiator ammonium persulfate after slurry exhaust, fully stir and inject die cavity after removing bubble, adding catalyzer Tetramethyl Ethylene Diamine, gelation 30 ~ 60min, place after the demoulding and steadily locates;
(4) base substrate is put into baking oven, temperature is 60 ~ 80 DEG C, drying time 8 ~ 12h;
(5), after drying, at 400 ~ 700 DEG C of removing forming agents that come unstuck, obtain precast body, then surface working, precision reaches sealing material level;
(6) above-mentioned precast body is put into Reaktionsofen, under vacuum atmosphere, be warming up to temperature of reaction, pass into certain trichloromethyl silane, hydrogen is as carrier gas, argon gas is as diluent gas, and temperature of reaction is 1000 ~ 1200 DEG C, and trichloromethyl silane flow is 30 ~ 50sccm, hydrogen flowing quantity is 200 ~ 300sccm, argon flow amount is 200 ~ 300sccm, controls reaction conditions, chemical vapor infiltration silicon carbide whisker, precast body densification, penetration time is 200 ~ 300h;
(7) complete densification post-treatment to original surface accuracy, finally obtain the ceramic base composition board of SiC whisker reinforcement.
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| CN106915975A (en) * | 2015-12-25 | 2017-07-04 | 苏州宏久航空防热材料科技有限公司 | The preparation method of carbon materials surface SiC-C coatings in graphite heater stove |
| CN109704771B (en) * | 2019-01-17 | 2021-11-19 | 宁波伏尔肯科技股份有限公司 | Preparation method of boron carbide porous ceramic for high-temperature gas cooled reactor nuclear control rod |
| CN110428918B (en) * | 2019-08-08 | 2021-07-20 | 中国核动力研究设计院 | Rapid densification method and device for high-density composite material cladding tube |
| CN112030544B (en) * | 2020-08-31 | 2021-06-15 | 北京航空航天大学 | Method for in-situ growth of silicon carbide nanowires on surface of silicon carbide fiber |
| CN113285146B (en) * | 2021-07-22 | 2021-10-08 | 华东交通大学 | Electric vehicle battery heat preservation device and method |
| CN114804819B (en) * | 2022-06-14 | 2023-04-07 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant aerogel composite material and composite material thereof |
| CN115231937B (en) * | 2022-07-04 | 2023-08-01 | 武汉科技大学 | B 4 Composite ceramic powder for in-situ generation of SiC whisker on C surface and preparation method thereof |
| CN116200626B (en) * | 2023-03-23 | 2023-11-10 | 哈尔滨工业大学 | In-situ preparation method of diamond and silicon carbide mixed reinforced high-heat-conductivity high-strength aluminum-based composite material |
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|---|---|---|---|---|
| CN101037336A (en) * | 2007-04-29 | 2007-09-19 | 北京科技大学 | Method for preparing carborundum whisker reinforced carborundum composite material element |
| CN101798182A (en) * | 2010-02-04 | 2010-08-11 | 西北工业大学 | Preparation method of laminated ceramic composite |
| CN101941231A (en) * | 2010-09-09 | 2011-01-12 | 中国科学院长春光学精密机械与物理研究所 | Gel injection molding technology of large-sized and complicated-shape silicon carbide ceramic biscuit |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037336A (en) * | 2007-04-29 | 2007-09-19 | 北京科技大学 | Method for preparing carborundum whisker reinforced carborundum composite material element |
| CN101798182A (en) * | 2010-02-04 | 2010-08-11 | 西北工业大学 | Preparation method of laminated ceramic composite |
| CN101941231A (en) * | 2010-09-09 | 2011-01-12 | 中国科学院长春光学精密机械与物理研究所 | Gel injection molding technology of large-sized and complicated-shape silicon carbide ceramic biscuit |
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