CN100457682C - Compact foamy thyrite in high intensity and preparation method - Google Patents
Compact foamy thyrite in high intensity and preparation method Download PDFInfo
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- CN100457682C CN100457682C CNB031340393A CN03134039A CN100457682C CN 100457682 C CN100457682 C CN 100457682C CN B031340393 A CNB031340393 A CN B031340393A CN 03134039 A CN03134039 A CN 03134039A CN 100457682 C CN100457682 C CN 100457682C
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Abstract
The invention provides a high strength compact foam silicon carbide ceramics material and the prodn method. Counting on weight percentage, the material is composed by silicon carbide 90-98 and silicon 10-2, silicon carbide powder and resin with high carbon-producing ration are mixed to slurry, expanded plastice is cut and soaked in the slurry, which is taken out, removing unnecessary slurry, then is treated by semisolidifying, high-temp, high-pressure solidifying, the solidified foam body is pyrolized to obtain foam carbon frame with same shape as original foam shape composed by silicon carbide and pylolized carbon, to open a centre hole on carbon frame by grinding, the silicon slurry is injected into the centre hole until filling by press injection, then is pylolized, by silicizing process, carbon in the carbon frame and gas or liquid phase silicen are reacted to generate silicon carbide and combined with original silicon carbide particles in carbon frame, thus to obtain high strength compact silicon carbide foam ceramics.
Description
Technical field
The present invention relates to the foam silicon carbon stupalith, specifically foam silicon carbon stupalith of a kind of high strength dense and preparation method thereof.
Background technology
Foamed ceramics is a kind of special porous ceramics.Its geometry feature is to be elementary cell with polygonal Closed loop, the three-dimensional networks that each elementary cell is interconnected to form.Because silicon carbide has excellent high temperature resistant, anti-oxidant, acid-alkali-corrosive-resisting, thermal shock resistance and characteristic of semiconductor, the making and the application of foam silicon carbon pottery are paid attention to widely.
Present foam silicon carbon pottery has following four kinds of methods preparation: powder sintering, solid state reaction sintering process, contain silicone resin pyrolysis method and vapour deposition process.
Powder sintering is divided into two kinds of different processes again.After the first will contain the slip of the carborundum powder of a certain amount of sintering aid and linking agent (as ethyl silicate hydrolyzed solution, silicon sol etc.) furnishing suitable concn, soak and hang on the polyurethane foam, after solidifying drying, deviate from linking agent and polyurethane foam 200～600 ℃ of scopes.Then, temperature is elevated to carries out sintering between 1500～2200 ℃ and just obtain foamed silicon carbide ceramics; Another kind method is with after containing the carborundum powder and strain shape whipping agent uniform mixing of sintering aid, with mold pressing or pouring procedure moulding.Deviate from whipping agent by fusing or gasification, carry out high temperature sintering then to obtain the spumescence silicon carbide ceramics.
The solid state reaction sintering process is with strain shape whipping agent and silica flour and the moulding of carbon dust uniform mixing.Deviate from whipping agent by fusing or gasification, through promptly obtaining the spumescence silicon carbide ceramics behind the pyroreaction sintering.
Containing the silicone resin pyrolysis method is that the organosilicon presoma is made high-molecular gel, obtains the foamed silicone resin that contains after deviating from the organic solvent in the gel, carries out pyrolysis and promptly obtain the spumescence silicon carbide ceramics after fully giving oxidation.
To be the method for utilizing chemical vapour deposition with silicon carbide deposit on the netlike carbon fiber knitted body vapour deposition process and obtain the spumescence silicon carbide ceramics.
Too high cost of manufacture makes CVD (Chemical Vapor Deposition) method lose the possibility of industrial-scale production foam silicon carbon pottery basically.With other foamed ceramics (as aluminum oxide, zirconium white), intensity is low to be the common basic problems that exist of existing various foam silicon carbon ceramic preparations always.Except that the foam silicon carbon pottery of gas phase deposition method preparation, the low basic reason of foam silicon carbon ceramics strength of other method preparation be constitute the density of ceramic muscle of foamed ceramics skeleton not high due to.
A kind of high-strength foam silicon carbide ceramics that the present patent application person proposes in Chinese invention patent application (application number is 00110479.9) and preparation method thereof, the relative density of ceramic muscle is reached more than 90%, thereby improve the intensity of foam silicon carbon pottery significantly.Research work in recent years finds that remaining silicone content too high (generally surpassing 20%), skewness have limited the raising of foam silicon carbon ceramics strength in the ceramic muscle, remain further to be solved.
Summary of the invention
The object of the present invention is to provide foam silicon carbon stupalith of a kind of high strength dense and preparation method thereof, ceramic muscle density height (surpassing 99%), remaining silicone content low (less than 10%), homogeneous microstructure with the foam silicon carbon pottery of this method preparation are significantly improved the intensity of foam silicon carbon pottery.
Technical scheme of the present invention is:
A kind of high strength dense foam silicon carbon foam ceramic material is characterized in that: mark meter by weight, its composition is made up of 90%～98% silicon carbide and 10%～2% silicon.
Wherein said foam silicon carbide ceramics is an elementary cell with polygonal Closed loop, and each elementary cell is interconnected to form three-dimensional networks; Constitute relative density 〉=99% of the unitary ceramic muscle of Polygons Closed loop, average grain size is at 50nm～10 μ m.
A kind of preparation method of described compact silicon carbide foamed ceramics is characterized in that: with carborundum powder, high carbon output rate resin is basic raw material, is template with the porous plastics, and preparation process is as follows:
1) slip preparation
Carborundum powder, high carbon output rate resin, solidifying agent and ethanol are mixed in proportion, weight percent is 80wt%～30wt%: 19wt%～50wt%: 1wt%～20wt% between carborundum powder, high carbon output rate resin and the solidifying agent, 0.5～2 hour ball milling time after mechanical stirring, filter through 35～140 eye mesh screens, get slip, the weight of solid substance in the described slip (be solute, comprise: carborundum powder, high carbon output rate resin and solidifying agent) is 30～80% of slip total amount;
2) soak extension
Foam is cut into desired shape and size, immerses equably in the slip, squeeze after taking out and remove unnecessary slip, adopt air-blowing and centrifugal mode to remove unnecessary slip, heating semicure, 50～80 ℃ of Heating temperatures, set time, 5～60min obtained the foam silicon carbon ceramic forerunner;
3) hot-pressing densification
The foam silicon carbide ceramics presoma is put into high pressure vessel, charge into nitrogen or rare gas element and carry out high temperature, high pressure and solidify, pressure be 1～35MPa, temperature at 50～300 ℃, 1～5 ℃ of heat-up rate, be incubated 5 minutes～3 hours, obtain fine and close foam silicon carbon foamed ceramics presoma;
4) pyrolysis
With foam silicon carbide ceramics presoma pyrolysis under the protection of nitrogen or inert atmosphere of densification, 1～5 ℃ of temperature rise rate per minute is warming up to 600～1300 ℃, is incubated 0.5～2 hour, obtains the foamed ceramics carbon skeleton;
5) fill the carbon skeleton centre hole
Because foam is burnt after the pyrolysis, stays centre hole in foamed ceramics carbon skeleton muscle, therefore need to fill the carbon skeleton centre hole, realize densification.After the centre hole on carbon skeleton surface mill opened, utilizing the method for high pressure pressure injection will fill slip is pressed in the centre hole, pressure is 1～35MPa, pressurize 10 minutes～2 hours, obtain fine and close foam silicon carbon carbon skeleton through pyrolysis, pyrolysis is carried out under nitrogen or inert atmosphere or vacuum condition, temperature rise rate is 1～10 ℃ of a per minute, and 600～1300 ℃ of temperature are incubated 0.5～2 hour;
6) siliconising
Sic foam carbon skeleton reaction sintering siliconising with the densification after the pyrolysis, siliconising is carried out under nitrogen or inert atmosphere or vacuum condition, and temperature rise rate is 5～15 ℃ of per minutes, and temperature is: 1400～2000 ℃, be incubated 0.5～4 hour, get high strength dense foam silicon carbon stupalith.
Described high carbon output rate resin is selected from one or more of Resins, epoxy, resol, furfuryl resin, phenol-furfural resin.
Described alcohol concn is 〉=95%.
It is the carborundum powder of 10nm～15 μ m that described carborundum powder adopts mean particle size.
Described solidifying agent is that one of product, oxalic acid or citric acid are taken off in tosic acid, five Lip rivers.
Described porous plastics is polyurethane porous plastics or polyether ester porous plastics, and its aperture is 1～3mm.
The present invention makes slip with carborundum powder and high carbon output rate mixed with resin; Select the porous plastics in suitable aperture, and be cut into needed shape and size, then it is immersed in slip, after the taking-up, remove unnecessary slip, semicure with extruding, wind, mode such as centrifugal; High temperature, high pressure solidify in high pressure vessel, to improve the initial density of foamed ceramics skeleton presoma; Foams after solidifying are carried out pyrolysis in vacuum or rare gas element or nitrogen protection stove, obtain the same with the original foam shape spumescence carbon skeleton of forming by silicon carbide and RESEARCH OF PYROCARBON; The carbon skeleton centre hole left by mill, with the pressure injection method with silicon carbide slip pressure injection in the carbon skeleton centre hole and add full centre hole, pyrolysis then; Through the siliconising process, the carbon in the carbon skeleton and gas phase or liquid-phase silicone reaction generation silicon carbide, and combine with original silicon-carbide particle in the foam framework, thus obtain the foam silicon carbide ceramics of high strength dense.
The present invention has following beneficial effect:
1, ceramic muscle density height, even, the remaining silicon amount of microstructure are few.
The present invention adopts the method for hot-press solidifying foamed ceramics skeleton presoma, has not only significantly improved the initial density of foamed ceramics presoma muscle, has also eliminated repeatedly to soak and has hung the layering that forms and the microstructure problem of non-uniform that causes; And utilize the pressure injection method to force the silicon carbide slip to enter in the foamed ceramics carbon skeleton centre hole, and, make to be full of silicon carbide in the centre hole by the siliconising reaction.The employing of these two measures makes that the density of ceramic muscle remains on more than 99%, remaining silicone content reduces to (generally below 5%) below 10%, microstructure is very even, sees accompanying drawing 1,2,3.This is the not available distinguishing feature of other foam silicon carbon ceramic preparation.
2, intensity height.
Increase substantially and the minimizing significantly of remaining silicon amount amount because ceramic muscle density, microstructure be inhomogeneity, fundamentally solved the low key reason of foamed ceramics intensity, made the ratio ultimate compression strength of the foam silicon carbon pottery that the present invention prepares reach 500MPacm
3G
-1Ratio ultimate compression strength than the foam silicon carbon pottery of the method preparation that proposes at Chinese invention patent (application number is 00110479.9) with the present patent application person improves more than 2 times, than 5～10 times of the ratio ultimate compression strength raisings of the foam silicon carbon pottery for preparing with other method.
Description of drawings
Fig. 1 is the macro morphology (scale is 1mm) of foam silicon carbon pottery.
Fig. 2 is the fracture apperance (scale is 200 μ m) of foam silicon carbon pottery muscle.
Fig. 3 is the microstructure (scale is 50 μ m) of foam silicon carbon pottery muscle inside.
Embodiment
Below by embodiment in detail the present invention is described in detail.
Embodiment 1
Weight ratio is respectively 60%: 35%: 5% mean particle size 2 μ m carborundum powders, ammonia resol, tosic acid is dissolved in the dehydrated alcohol altogether, make solid substance in the slip: carborundum powder, the weight of high carbon output rate resin and solidifying agent is 40% of slip total amount, the 0.5 hour ball milling time after mechanical stirring, filter through 35 eye mesh screens, make slip, the polyurethane foam of aperture 1mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, semicure is carried out in air-dry back in baking oven, 50 ℃ of temperature, 10 minutes time.The said process repeated multiple times is up to reaching the required weight of 30% pre-determined volume mark (volume fraction of silicon carbide ceramics in the finished product).Then, put into high pressure vessel, charge into nitrogen and make air pressure reach 12MPa, be warming up to 250 ℃, 2 ℃ of heat-up rate per minutes are incubated curing in 1 hour, obtain presoma.With presoma pyrolysis under argon shield, generate carbon skeleton; Wherein the temperature rise rate per minute is 2 ℃, is warming up to 800 ℃, is incubated 0.5 hour.The centre hole on carbon skeleton surface mill is opened, and in high pressure vessel, is that the slip of 150mPas is pressed in the centre hole with viscosity, and pressure is 5Mpa, and pressurize is after 20 minutes, pyrolysis under argon shield, and temperature rise rate is 2 ℃ of per minutes, 800 ℃ of temperature are incubated 0.5 hour; After the pyrolysis, carry out the vacuum siliconising, temperature rise rate is 10 ℃/minute, 1800 ℃ of temperature are incubated 1 hour, get the high strength dense silicon carbide foam ceramic material, the muscle density is 99%, remaining silicone content 5%, silicon carbide average crystal grain granularity is 1.8 μ m, the foam silicon carbon pottery is than ultimate compression strength 460MPacm
3G
-1, its composition is a silicon carbide: 98%, and silicon: 2%.
Embodiment 2
Difference from Example 1 is:
Weight ratio is respectively 45%: 50%: 5% mean particle size 2 μ m carborundum powders, Resins, epoxy (trade mark is EP0141-310), tosic acid is dissolved in the dehydrated alcohol altogether, make solid substance in the slip: carborundum powder, the weight of high carbon output rate resin and solidifying agent is 60% of slip total amount, the 1 hour ball milling time after mechanical stirring, filter through 55 eye mesh screens, make slip, the polyurethane foam of aperture 2mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, after air-dry, 50 ℃ of following semicures 10 minutes, the said process repeated multiple times is up to reaching the required weight of 20% pre-determined volume mark (volume fraction of silicon carbide ceramics in the finished product).Then, put into high pressure vessel, charge into nitrogen and make air pressure reach 10MPa, be warming up to 200 ℃, 3 ℃ of heat-up rate per minutes are incubated curing in 1 hour.Pyrolysis under argon shield generates carbon skeleton; Wherein the temperature rise rate per minute is 2 ℃, is warming up to 900 ℃, is incubated 0.5 hour.The centre hole on carbon skeleton surface mill is opened, and in high pressure vessel, is that the slip of 200mPas is pressed in the centre hole with viscosity, and pressure is 10Mpa, and pressurize is after 40 minutes, pyrolysis under argon shield, and temperature rise rate is 3 ℃ of per minutes, 900 ℃ of temperature are incubated 1 hour; After the pyrolysis, carry out the vacuum siliconising, 1600 ℃ of temperature of reaction, temperature rise rate is 10 ℃/minute, be incubated 1 hour, get the high strength dense silicon carbide foam ceramic material, the muscle density is 99%, silicon carbide average crystal grain granularity is 1.7 μ m, and its composition is a silicon carbide: 95%, and silicon: 5%.
Embodiment 3
Difference from Example 1 is:
Carborundum powder, resin (heat-reactive phenolic resin 30%, furfuryl resin 70%) and oxalic acid weight ratio are 70wt%: 20wt%: 10wt%, be dissolved in heat-reactive phenolic resin, furfuryl resin and oxalic acid in the dehydrated alcohol altogether, make slurry solution, the carborundum powder that with mean particle size is 5 μ m more evenly adds in the above-mentioned solution, make solid substance in the slip: the weight of carborundum powder, high carbon output rate resin and solidifying agent is 50% of slip total amount, the 2 hours ball milling time after mechanical stirring, filter through 75 eye mesh screens, make slip.The polyurethane foam of aperture 2mm cut into require to immerse equably in the described slip after the size, squeeze after taking out and remove unnecessary slip, soaked 1 minute, air-dry back 60 ℃ of semicures 50 minutes, the said process repeated multiple times is up to reaching the required weight of 40% pre-determined volume mark (volume fraction of silicon carbide ceramics in the finished product).Put into high pressure vessel, charge into nitrogen and make air pressure reach 11MPa, be warming up to 230 ℃, 4 ℃ of heat-up rate per minutes are incubated curing in 15 minutes.Pyrolysis under nitrogen protection generates carbon skeleton; Wherein the temperature rise rate per minute is 3 ℃, is warming up to 1000 ℃, is incubated 1 hour.The centre hole on carbon skeleton surface mill is opened, and in high pressure vessel, is that the slip of 250mPas is pressed in the centre hole with viscosity, and pressure is 15Mpa, and pressurize is after 1 hour, pyrolysis under nitrogen protection, and temperature rise rate is 6 ℃ of per minutes, 1000 ℃ of temperature are incubated 2 hours; After the pyrolysis, under nitrogen protection, carry out siliconising, 1650 ℃ of temperature of reaction, temperature rise rate is 15 ℃/minute; be incubated 2 hours, get the high strength dense silicon carbide foam ceramic material, the muscle density is 99%; silicon carbide average crystal grain granularity is 4.2 μ m, and its composition is a silicon carbide: 92%, and silicon: 8%.
Embodiment 4
Difference from Example 1 is:
Weight ratio is respectively 60%: 35%: 5% mean particle size 1.5 μ m carborundum powders, boron bakelite resin, five Lip rivers are taken off product and are dissolved in the dehydrated alcohol altogether, make solid substance in the slip: carborundum powder, the weight of high carbon output rate resin and solidifying agent is 80% of slip total amount, the 0.5 hour ball milling time after mechanical stirring, filter through 95 eye mesh screens, make slip, the polyurethane foam of aperture 2mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, air-dry back 80 ℃ of semicures 20 minutes, the said process repeated multiple times is up to reaching the required weight of 50% pre-determined volume mark (volume fraction of silicon carbide ceramics in the finished product).Put into high pressure vessel, charge into argon gas and make air pressure reach 18MPa, be warming up to 260 ℃, 5 ℃ of heat-up rate per minutes are incubated curing in 2 hours.Pyrolysis under argon shield generates carbon skeleton; Wherein the temperature rise rate per minute is 4 ℃, is warming up to 600 ℃, is incubated 2 hours.The centre hole on carbon skeleton surface mill is opened, and in high pressure vessel, is that the slip of 300mPas is pressed in the centre hole with viscosity, and pressure is 35Mpa, and pressurize is after 10 minutes, pyrolysis under argon shield, and temperature rise rate is 8 ℃ of per minutes, 1200 ℃ of temperature are incubated 0.5 hour; After the pyrolysis; under argon shield, carry out siliconising; 1400 ℃ of temperature of reaction; temperature rise rate is 5 ℃/minute, is incubated 3 hours, gets the high strength dense silicon carbide foam ceramic material; the muscle density is 100%; silicon carbide average crystal grain granularity is 1.1 μ m, and its composition is a silicon carbide: 90%, and silicon: 10%.
Embodiment 5
Difference from Example 1 is:
Carborundum powder, resin (heat-reactive phenolic resin 60%, furfuryl resin 40%) and to take off the product weight ratio be 50wt%: 30wt%: 20wt% in five Lip rivers, product are taken off in heat-reactive phenolic resin and furfuryl resin and five Lip rivers to be dissolved in the dehydrated alcohol altogether, make slurry solution, the carborundum powder that with mean particle size is 5 μ m more evenly adds in the above-mentioned solution, make solid substance in the slip: carborundum powder, the weight of high carbon output rate resin and solidifying agent is 30% of slip total amount, the 1 hour ball milling time after mechanical stirring, filter through 120 eye mesh screens, make slip, the polyurethane foam of aperture 2mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, air-dry back 50 ℃ of semicures 30 minutes, the said process repeated multiple times is up to reaching the required weight of 60% pre-determined volume mark (volume fraction of silicon carbide ceramics in the finished product).Put into high pressure vessel, charge into nitrogen and make air pressure reach 25MPa, be warming up to 240 ℃, 2 ℃ of heat-up rate per minutes are incubated curing in 1 hour.Pyrolysis under argon shield generates carbon skeleton; Wherein the temperature rise rate per minute is 4 ℃, is warming up to 1000 ℃, is incubated 0.5 hour.The centre hole on carbon skeleton surface mill is opened, and in high pressure vessel, is that the slip of 180mPas is pressed in the centre hole with viscosity, and pressure is 20Mpa, and pressurize is after 2 hours, pyrolysis under argon shield, and temperature rise rate is 6 ℃ of per minutes, 600 ℃ of temperature are incubated 2 hours; After the pyrolysis, carry out the vacuum siliconising, 1550 ℃ of temperature of reaction, temperature rise rate is 15 ℃/minute, be incubated 1 hour, get the high strength dense silicon carbide foam ceramic material, the muscle density is 99%, silicon carbide average crystal grain granularity is 3.8 μ m, and its composition is a silicon carbide: 96%, and silicon: 4%.
Embodiment 6
Difference from Example 1 is:
Carborundum powder, resin (heat-reactive phenolic resin 50%, furfuryl resin 50%) and the citric acid weight ratio be 40wt%: 40wt%: 20wt%, be dissolved in heat-reactive phenolic resin and furfuryl resin and citric acid in the dehydrated alcohol altogether, make slurry solution, the carborundum powder that with mean particle size is 10 μ m more evenly adds in the above-mentioned solution, make solid substance in the slip: carborundum powder, the weight of high carbon output rate resin and solidifying agent is 80% of slip total amount, the 2 hours ball milling time after mechanical stirring, filter through 140 eye mesh screens, make slip, the polyurethane foam of aperture 3mm cut into require to immerse equably in the described slip after the size, soaked 1 minute, squeeze after taking out and remove unnecessary slip, air-dry back 50 ℃ of semicures 10 minutes, the said process repeated multiple times is up to reaching the required weight of 10% pre-determined volume mark (volume fraction of silicon carbide ceramics in the finished product).Put into high pressure vessel, charge into nitrogen and make air pressure reach 20MPa, be warming up to 280 ℃, 5 ℃ of heat-up rate per minutes are incubated curing in 1 hour.Pyrolysis under argon shield generates carbon skeleton; Wherein the temperature rise rate per minute is 2 ℃, is warming up to 900 ℃, is incubated 0.5 hour.The centre hole on carbon skeleton surface mill is opened, and in high pressure vessel, is that the slip of 280mPas is pressed in the centre hole with viscosity, and pressure is 30Mpa, and pressurize is after 30 minutes, pyrolysis under argon shield, and temperature rise rate is 5 ℃ of per minutes, 800 ℃ of temperature are incubated 2 hours; After the pyrolysis, carry out the vacuum siliconising, 1650 ℃ of temperature of reaction, temperature rise rate is 15 ℃/minute, be incubated 1 hour, get the high strength dense silicon carbide foam ceramic material, the muscle density is 100%, silicon carbide average crystal grain granularity is 7.2 μ m, and its composition is a silicon carbide: 94%, and silicon: 6%.
Claims (7)
1. high strength dense silicon carbide foam ceramic material is characterized in that: mark meter by weight, and its composition is made up of 90%～98% silicon carbide and 10%～2% silicon; Constitute relative density 〉=99% of the unitary ceramic muscle of Polygons Closed loop, average grain size is at 50nm～10 μ m.
2. preparation method by the described compact silicon carbide foamed ceramics of claim 1, it is characterized in that: with carborundum powder, high carbon output rate resin is basic raw material, is template with the porous plastics, and preparation process is as follows:
1) slip preparation
Carborundum powder, high carbon output rate resin, solidifying agent and ethanol are mixed in proportion, weight percent is 80wt%～30wt%: 19wt%～50wt%: 1wt%～20wt% between carborundum powder, high carbon output rate resin and the solidifying agent, 0.5～2 hour ball milling time after mechanical stirring, filter through 35～140 eye mesh screens, get slip, the weight of solid substance is 30～80% of slip total amount in the described slip;
2) soak extension
Foam is cut into desired shape and size, immerses equably in the slip, squeeze after taking out and remove unnecessary slip, adopt air-blowing and centrifugal mode to remove unnecessary slip, heating semicure, 50～80 ℃ of Heating temperatures, set time, 5～60min obtained the foam silicon carbon ceramic forerunner;
3) hot-pressing densification
The foam silicon carbide ceramics presoma is put into high pressure vessel, charge into nitrogen or rare gas element and carry out high temperature, high pressure and solidify, pressure be 1～35MPa, temperature at 50～300 ℃, 1～5 ℃ of heat-up rate, be incubated 5 minutes～3 hours, obtain fine and close foam silicon carbon foamed ceramics presoma;
4) pyrolysis
With foam silicon carbide ceramics presoma pyrolysis under the protection of nitrogen or inert atmosphere of densification, 1～5 ℃ of temperature rise rate per minute is warming up to 600～1300 ℃, is incubated 0.5～2 hour, obtains the foamed ceramics carbon skeleton;
5) fill the carbon skeleton centre hole
After the centre hole on carbon skeleton surface mill opened, utilizing the method for high pressure pressure injection will fill slip is pressed in the centre hole, pressure is 1～35MPa, pressurize 10 minutes～2 hours, obtain fine and close foam silicon carbon carbon skeleton through pyrolysis, pyrolysis is carried out under nitrogen or inert atmosphere or vacuum condition, temperature rise rate is 1～10 ℃ of a per minute, and 600～1300 ℃ of temperature are incubated 0.5～2 hour;
6) siliconising
Sic foam carbon skeleton reaction sintering siliconising with the densification after the pyrolysis, siliconising is carried out under nitrogen or inert atmosphere or vacuum condition, and temperature rise rate is 5～15 ℃ of per minutes, and temperature is: 1400～2000 ℃, be incubated 0.5～4 hour, get high strength dense foam silicon carbon stupalith.
3. according to the preparation method of the described compact silicon carbide foam ceramic material of claim 2, it is characterized in that: described high carbon output rate resin is selected from one or more of Resins, epoxy, resol, furfuryl resin, phenol-furfural resin.
4. according to the preparation method of the described compact silicon carbide foam ceramic material of claim 2, it is characterized in that: described alcohol concn is 95%.
5. according to the preparation method of the described compact silicon carbide foam ceramic material of claim 2, it is characterized in that: it is the carborundum powder of 10nm～15 μ m that described carborundum powder adopts mean particle size.
6. according to the preparation method of the described dense foam thyrite of claim 2, it is characterized in that: described solidifying agent is that one of product, oxalic acid or citric acid are taken off in tosic acid, five Lip rivers.
7. according to the preparation method of the described dense foam thyrite of claim 2, it is characterized in that: described porous plastics is polyurethane porous plastics or polyether ester porous plastics, and its aperture is 1～3mm.
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| US5195843A (en) * | 1991-05-30 | 1993-03-23 | Minnesota Mining And Manufacturing Company | Ceramic foam body having closed cell structure |
| CN1325832A (en) * | 2000-05-31 | 2001-12-12 | 中国科学院金属研究所 | High-strength foam silicon carbide ceramics and its preparing process |
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