CN104119094A - SiC whisker-reinforced ceramic-based composite plate and preparation method thereof - Google Patents
SiC whisker-reinforced ceramic-based composite plate and preparation method thereof Download PDFInfo
- Publication number
- CN104119094A CN104119094A CN201410391803.4A CN201410391803A CN104119094A CN 104119094 A CN104119094 A CN 104119094A CN 201410391803 A CN201410391803 A CN 201410391803A CN 104119094 A CN104119094 A CN 104119094A
- Authority
- CN
- China
- Prior art keywords
- ceramic
- sic whisker
- sic
- composition board
- ceramic powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a SiC whisker-reinforced ceramic-based composite plate and a preparation method thereof. The SiC whisker-reinforced ceramic-based composite plate comprises the following raw materials by volume percent: 60%-80% of inorganic ceramic powder substrate and 20%-40% of chemical vapor infiltration (CVI)-SiC whiskers, wherein the SiC whiskers are inlaid in the ceramic substrate and are closely combined with the ceramic substrate; the inorganic ceramic powder substrate is silicon carbide, silicon nitride, boron nitride or boron carbide, and the particle size of ceramic powder is 10-100m um. A ceramic preform is prepared by adopting a gel casting method, and the SiC whiskers grow in the preform in combination with a chemical vapor infiltration CVI process to densify the ceramic preform. The SiC whisker-reinforced ceramic-based composite plate is prepared by adopting combination of the gel casting process and CVI process, is improved in breaking tenacity and bending strength and is high in use reliability.
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 enhancing 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 that various countries are studied.
Silicon carbide whisker (SiC
w) be that a kind of diameter is that nano level is to the micron-sized single crystal fibre with height-oriented property, crystalline structure and diamond are 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 of >), 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 is to have 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.Utilizing it to carry out the larger stupalith of fragility toughness reinforcing, improve the performance of stupalith, be widely applied preparing aspect high performance composite, is also a kind of strongthener of studying morely for toughening ceramic based composites.
The method of producing at present 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 separating 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 is the organic gas that reacts or decompose a kind of carbon containing, silicon compound with carbonaceous gas with silicon-containing gas, synthetic SiC whisker, wherein chemical vapour deposition (CVD) is the most general with the application of chemical vapor infiltration (CVI) technology.The method has can control the silicon carbide whisker that generates 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 the Chinese patent of 201110122040.X SiC ceramic matric composite of disclosing the strengthening of a kind of SiC whisker and preparation method thereof, matrix material is prepared by Si or the reaction of Si alloy infiltration by prefabricated component, and described prefabricated component is made by the raw material compression molding that comprises SiC Whiskers from Rice Hulls product.Preparation technology is simple for this composite process, and infiltration temperature of reaction is low, and without impressed pressure, prefabricated component can be made into complicated shape, can be used for preparing complex shaped components.
Application number is the preparation technology that 201210088399.4 Chinese patent discloses the toughness reinforcing zirconium diboride pottery of a kind of silicon carbide whisker.Adopt sol-gel method at ZrB
2particle surface parcel SiO
2, after drying, grinding, add activated carbon fully to mix, compound heating under mobile argon gas atmosphere protection, utilizes SiO
2carbothermic reduction reaction between-C is at ZrB
2surface in situ generates SiC
w, obtain ZrB
2-SiC
wpowder, then sintering is prepared the toughness reinforcing zirconium diboride stupalith of silicon carbide whisker.Solve SiC
wdispersing uniformity problem in base material, has improved the structure of material, has improved the performance of material.
The silicon carbide whisker obtaining 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 meeting reduces the quality of silicon carbide whisker, has affected the enhancement of silicon carbide whisker to base material.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, ceramic base composition board of a kind of SiC whisker enhancing and preparation method thereof is provided, it is characterized in that the ceramic base composition board that described SiC whisker strengthens 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, side is tabular etc.Adopt the method for gel casting 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 to 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 enhancing, it is characterized in that, comprises following sequential steps:
(1) in the aqueous solution, add monomer acrylamide and linking agent methylene-bisacrylamide to form the premixed liquid that concentration is 10%～20%;
(2) in the good inorganic ceramic powder of proportioning, add premixed liquid and dispersion agent ammonium polyacrylate by 55%～60% solid volume component requirement, regulate PH to 9～11, ball milling mixes 10～20h, makes slurry;
(3) after slurry exhaust, add initiator ammonium persulfate, inject die cavity after fully stirring and remove bubble, add catalyzer Tetramethyl Ethylene Diamine, gelation 30～60min, places steadily place after the demoulding;
(4) above-mentioned base substrate is put into baking oven, temperature is 60～80 DEG C, drying time 8～12h;
(5) after dry, come unstuck and remove forming agent at 400～700 DEG C, 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 that SiC whisker strengthens.
The present invention has advantages of: 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
weven in matrix inner dispersion, and to combine closely, reinforced effects is better; 3, goods toughness improves, and fracture toughness property and flexural strength improve, and work reliability is high.
Brief description of the drawings
Fig. 1 is the sectional view of the ceramic base composition board of discoideus SiC whisker enhancing.
10 is inorganic ceramic powder base material; 20 is chemical vapor infiltration (CVI)-SiC whisker.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims to the amendment of the various equivalent form of values of the present invention and limit.
Embodiment 1
(1) in the aqueous solution, add monomer acrylamide and linking agent methylene-bisacrylamide to form the premixed liquid that concentration is 15%;
(2) in the good inorganic ceramic powder of proportioning, add premixed liquid and dispersion agent ammonium polyacrylate by 55% solid volume component requirement, regulate PH to 11, ball milling mixing 15h, makes slurry;
(3) after slurry exhaust, add initiator ammonium persulfate, inject die cavity after fully stirring and remove bubble, add catalyzer Tetramethyl Ethylene Diamine, gelation 45min, places steadily place after the demoulding;
(4) above-mentioned base substrate is put into baking oven, temperature is 70 DEG C, drying time 12h;
(5) after dry, come unstuck and remove forming agent at 600 DEG C, 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 that SiC whisker strengthens.
Embodiment 2
(1) in the aqueous solution, add monomer acrylamide and linking agent methylene-bisacrylamide to form the premixed liquid that concentration is 20%;
(2) in the good inorganic ceramic powder of proportioning, add premixed liquid and dispersion agent ammonium polyacrylate by 60% solid volume component requirement, regulate PH to 10, ball milling mixing 20h, makes slurry;
(3) after slurry exhaust, add initiator ammonium persulfate, inject die cavity after fully stirring and remove bubble, add catalyzer Tetramethyl Ethylene Diamine, gelation 60min, places steadily place after the demoulding;
(4) above-mentioned base substrate is put into baking oven, temperature is 80 DEG C, drying time 10h;
(5) after dry, come unstuck and remove forming agent at 700 DEG C, 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 that SiC whisker strengthens.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content that does not depart from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (6)
1. the ceramic base composition board that SiC whisker strengthens, is characterized in that comprising inorganic ceramic powder base material, SiC whisker, and SiC whisker is embedded in ceramic base material, and combines closely with ceramic base material.
2. composition board according to claim 1, is characterized in that inorganic ceramic powder base material volume fraction is that 60%～80%, SiC whisker is 20%～40%.
3. composition board according to claim 1, is characterized in that described inorganic ceramic powder base material is silicon carbide, silicon nitride, boron nitride, norbide.
4. composition board according to claim 1, is characterized in that described ceramic base composition board can be discoideus, square tabular.
5. composition board according to claim 1, is characterized in that described inorganic ceramic powder substrate ceramic powder particle size is 10～100um.
6. a preparation method for the ceramic base composition board that SiC whisker strengthens, is characterized in that comprising following sequential steps:
(1) in the aqueous solution, add monomer acrylamide and linking agent methylene-bisacrylamide to form concentration at 10%～20% premixed liquid;
(2) in the good inorganic ceramic powder of proportioning, add premixed liquid and dispersion agent ammonium polyacrylate by 55%～60% solid volume component requirement, regulate PH to 9～11, ball milling mixes 10～20h, makes slurry;
(3) after slurry exhaust, add initiator ammonium persulfate, inject die cavity after fully stirring and remove bubble, add catalyzer Tetramethyl Ethylene Diamine, gelation 30～60min, places steadily place after the demoulding;
(4) above-mentioned base substrate is put into baking oven, temperature is 60～80 DEG C, drying time 8～12h;
(5) after dry, come unstuck and remove forming agent at 400～700 DEG C, 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 that SiC whisker strengthens.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410391803.4A CN104119094B (en) | 2014-08-08 | 2014-08-08 | Ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410391803.4A CN104119094B (en) | 2014-08-08 | 2014-08-08 | Ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104119094A true CN104119094A (en) | 2014-10-29 |
| CN104119094B CN104119094B (en) | 2016-03-02 |
Family
ID=51764764
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410391803.4A Active CN104119094B (en) | 2014-08-08 | 2014-08-08 | Ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104119094B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109704771A (en) * | 2019-01-17 | 2019-05-03 | 宁波伏尔肯科技股份有限公司 | A kind of preparation method of high temperature gas cooled reactor nuclear control rod boron carbide porous ceramics |
| CN110428918A (en) * | 2019-08-08 | 2019-11-08 | 中国核动力研究设计院 | A kind of method for rapidly densifying and its device of high-compactness composite material cladding tubes |
| CN112030544A (en) * | 2020-08-31 | 2020-12-04 | 北京航空航天大学 | Method for in-situ growth of silicon carbide nanowires on surface of silicon carbide fiber |
| CN113285146A (en) * | 2021-07-22 | 2021-08-20 | 华东交通大学 | Electric vehicle battery heat preservation device and method |
| CN114804819A (en) * | 2022-06-14 | 2022-07-29 | 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 |
| CN115231937A (en) * | 2022-07-04 | 2022-10-25 | 武汉科技大学 | B 4 Composite ceramic powder for in-situ generation of SiC whiskers on C surface and preparation method thereof |
| CN116200626A (en) * | 2023-03-23 | 2023-06-02 | 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 |
Citations (3)
| 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 |
-
2014
- 2014-08-08 CN CN201410391803.4A patent/CN104119094B/en active Active
Patent Citations (3)
| 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 |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109704771A (en) * | 2019-01-17 | 2019-05-03 | 宁波伏尔肯科技股份有限公司 | A kind of preparation method of high temperature gas cooled reactor nuclear control rod boron carbide porous ceramics |
| CN110428918A (en) * | 2019-08-08 | 2019-11-08 | 中国核动力研究设计院 | A kind of method for rapidly densifying and its device of high-compactness composite material cladding tubes |
| CN112030544A (en) * | 2020-08-31 | 2020-12-04 | 北京航空航天大学 | Method for in-situ growth of silicon carbide nanowires on surface of silicon carbide fiber |
| 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 |
| CN113285146A (en) * | 2021-07-22 | 2021-08-20 | 华东交通大学 | Electric vehicle battery heat preservation device and method |
| CN113285146B (en) * | 2021-07-22 | 2021-10-08 | 华东交通大学 | Electric vehicle battery heat preservation device and method |
| CN114804819A (en) * | 2022-06-14 | 2022-07-29 | 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 |
| CN115231937A (en) * | 2022-07-04 | 2022-10-25 | 武汉科技大学 | B 4 Composite ceramic powder for in-situ generation of SiC whiskers on C surface and preparation method 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 |
| CN116200626A (en) * | 2023-03-23 | 2023-06-02 | 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 |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104119094B (en) | 2016-03-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104119094B (en) | Ceramic base composition board of a kind of SiC whisker reinforcement and preparation method thereof | |
| CN101555137B (en) | (TiB2+TiC)/Ti3SiC2Complex phase ceramic material and preparation method thereof | |
| CN106747530B (en) | Boron nitride nanosheet reinforced ceramic matrix composite and preparation method thereof | |
| CN103288468A (en) | Preparation method for fiber reinforced carbon-silicon carbide-zirconium carbide-based composite material | |
| CN103073320B (en) | Preparation method for ZrB2-SiC (w) ceramic raw material | |
| CN106167413B (en) | A kind of 90 aluminium oxide ceramics of On In-situ Synthesis of Mullite Whisker toughening and preparation method | |
| CN105272329B (en) | A kind of preparation method of alumina carbon SiClx zirconium carbide nano whisker enhancing cutting tool material | |
| CN105329895A (en) | Preparation method of silicon carbide nanometer crystal whiskers | |
| CN100363303C (en) | Silicon carbide base multiphase composite ceramic and its preparation method | |
| CN101555136B (en) | Titanium silicon carbide/titanium diboride-titanium carbide composite material and preparation method thereof | |
| WO2012165291A1 (en) | Method for producing silicon carbide-carbon composite | |
| CN105367058A (en) | Method of sintering high-toughness silicon carbide ceramic by using vacuum reaction | |
| CN105777172A (en) | Method for preparing Diamond/SiC composite material by combining thermally compression molding with chemical vapor infiltration (CVI) | |
| CN110436896B (en) | Method for preparing high-strength and high-toughness ceramic material by thermally cracking silica gel and inorganic filler compound | |
| JP3607945B2 (en) | Reactive synthesis of high-strength zirconium boride-silicon carbide composites | |
| JP5601833B2 (en) | Method for producing metal-ceramic composite material | |
| CN1844493A (en) | Method for synthesizing bionic silicon carbide crystal whisker | |
| CN107512921B (en) | Preparation method of carbon fiber powder reinforced silicon nitride-based composite material | |
| CN1296501C (en) | In-situ hot pressing process of synthesizing compact composite carbon titanosilicide-titanium diboride bulk material | |
| CN102126861A (en) | In-situ self-toughening ZrB2-based composite ceramic material and preparation method thereof | |
| KR100419778B1 (en) | Manufacturing method of silicon cabide-boron carbide composites by liquid phase reaction sintering | |
| CN111892411B (en) | Nitride-silicon carbide-calcium hexaluminate composite refractory product and preparation method thereof | |
| Ma et al. | Processing and characterization of particles reinforced SiOC composites via pyrolysis of polysiloxane with SiC or/and Al fillers | |
| JP4217278B2 (en) | Method for producing metal-ceramic composite material | |
| JP5300493B2 (en) | Intermetallic compound-containing composite and method for producing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |