CN110483053A - A kind of SiC nanowire/SiC porous ceramics preparation method for inhaling wave for high temperature - Google Patents
A kind of SiC nanowire/SiC porous ceramics preparation method for inhaling wave for high temperature Download PDFInfo
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Abstract
The present invention relates to SiC nanowire/SiC porous ceramics preparation methods, it in particular is a kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature, soluble silicon resin and catalyst is added during preparing ceramic green using gel injection-moulding method, in sintering, reaction in-situ generates SiC nanowire, the soluble silicon resin is to dissolve in the alcohols solvents such as ethyl alcohol, isopropanol and the tert-butyl alcohol, and the catalyst is ferrocene, FeCl3、Fe(NO3)3With Ni (NO3)2Equal metallic salts；Soluble silicon resin and catalyst can be added in Gel-casting process, direct in-situ reaction generates SiC nanowire in sintering；Organic siliconresin generates carbon and SiO2 after cracking, in the subsequent sintering process can in-situ preparation SiC nanowire, and then improve porous SiC mechanical property and absorbing property；The interconnected pore of the high-volume fractional formed after gel casting forming also promotes the V-L-S growth of SiC nanowire.
Description
Technical field
It is in particular a kind of for high temperature suction the present invention relates to SiC nanowire/SiC porous ceramics preparation method
The SiC nanowire of wave/SiC porous ceramics preparation method.
Background technique
SiC nanowire has very high specific strength, specific modulus, can reach effective enhancing, toughening in the composite
Effect, in addition, changing its also controllable electromagnetic performance of microscopic appearance of SiC nanowire.By the SiC for preparing diverse microcosmic appearance
Nano wire/SiC porous ceramics can get wide band wave transparent characteristic and excellent mechanical property.
Gel-casting process can be divided into water base and non-water base according to solvent for use difference.Aqueous gel casting is commonly used in system
Standby high-compactness ceramics, it is higher with gel strength prepared by water as solvent, but green body shrink in the drying process it is larger, it is difficult to make
Standby high stomata green body；With gel prepared by organic solvent, drying contraction is smaller, can be used for preparing high stomata green body, but having
The gel polymerisation degree prepared in solvent is low, and blank strength is low, is not easy to industrial production.
Summary of the invention
The object of the present invention is to provide it is a kind of for high temperature inhale wave SiC nanowire/SiC porous ceramics preparation method,
The integration system that SiC nanowire/SiC porous ceramics can be achieved is standby, improves the mechanical property and absorbing property of porous SiC.
The purpose of the present invention is achieved through the following technical solutions:
A kind of SiC nanowire/SiC porous ceramics preparation method for inhaling wave for high temperature, is prepared using gel injection-moulding method
Soluble silicon resin and catalyst are added during ceramic green, reaction in-situ generates SiC nanowire in sintering.
As advanced optimizing for the technical program, a kind of SiC nanowire/SiC for inhaling wave for high temperature of the present invention is porous
Ceramics preparation method, the preparation method the following steps are included:
Step 1: SiC powder and sintering aid ball milling mixing 12~for 24 hours, ball-milling medium is ethyl alcohol, mistake after ball milling drying
100~200 meshes；
Step 2: solvent, ceramic powder, dispersing agent, monomer, crosslinking agent, soluble silicon resin and catalyst ball milling are mixed
Conjunction 12~form slurry for 24 hours；
Step 3: mixed slurry being placed in vacuum and stirs de-bubble 10min, then initiator is added in the slurry and urges
Agent stirs injection molding after 10min, and is heated to 50~60 DEG C of heat preservation 0.5~2h gels；
Step 4: in the drying in 50~60 DEG C of baking oven after green body demoulding, 200 DEG C of heat preservations are heated to after being completely dried
2h makes the silicone resin crosslinking curing in green body；
Step 5: green body is placed in dumping in pyrolysis furnace；
Step 6: the green body after cracking dumping is placed in air pressure furnace and is sintered.
As advanced optimizing for the technical program, a kind of SiC nanowire/SiC for inhaling wave for high temperature of the present invention is porous
The volume ratio of the preparation method of ceramics, the ceramic powder and solvent is 1:1.5~9, the mass ratio of dispersing agent and ceramic powder
For 1:49~124, the mass ratio of monomer and ceramic powder is 1:6~33, and the mass ratio of crosslinking agent and monomer is 1:20~30, can
The mass ratio of dissolubility silicone resin and ceramic powder is 1:19~99, and the mass ratio of catalyst and solvent is 1:97~99.9.
As advanced optimizing for the technical program, a kind of SiC nanowire/SiC for inhaling wave for high temperature of the present invention is porous
The preparation method of ceramics, the solvent are ethyl alcohol, isopropanol and the tert-butyl alcohol, and dispersing agent is polyvinylpyrrolidone, monomer third
Acrylamide, crosslinking agent N, N- methylene-bisacrylamide, the soluble silicon resin are to dissolve in ethyl alcohol, isopropanol and uncle
Butanol, the catalyst are ferrocene, FeCl3、Fe(NO3)3With Ni (NO3)2。
As advanced optimizing for the technical program, a kind of SiC nanowire/SiC for inhaling wave for high temperature of the present invention is porous
The preparation method of ceramics, the sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio be 1:0.6~
0.8。
As advanced optimizing for the technical program, a kind of SiC nanowire/SiC for inhaling wave for high temperature of the present invention is porous
The preparation method of ceramics, the initiator being added in the slurry are ammonium persulfate, and the catalyst being added in slurry is tetramethyl second
Diamines.
As advanced optimizing for the technical program, a kind of SiC nanowire/SiC for inhaling wave for high temperature of the present invention is porous
The preparation method of ceramics, the mass ratio of the initiator and monomer are 1:3~10, the mass ratio of catalyst and monomer be 1:30~
200。
As advanced optimizing for the technical program, a kind of SiC nanowire/SiC for inhaling wave for high temperature of the present invention is porous
The preparation method of ceramics, the dump temperature are 550~650 DEG C, and heating rate is 0.3 DEG C/min, soaking time 2h, and atmosphere is
Nitrogen or argon gas.
As advanced optimizing for the technical program, a kind of SiC nanowire/SiC for inhaling wave for high temperature of the present invention is porous
The preparation method of ceramics is first warming up to 1500 DEG C of 0.5~1h of heat preservation with 10 DEG C/min the step of the sintering, then with 5 DEG C/
Min is warming up to 1700~1900 DEG C of 1~4h of heat preservation, and the sintering atmosphere is argon gas, and pressure is 0.4~1MPa.
As advanced optimizing for the technical program, a kind of SiC nanowire/SiC for inhaling wave for high temperature of the present invention is porous
The mass ratio of the preparation method of ceramics, the SiC powder and sintering aid is 1:89~99.
A kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature of the present invention has the beneficial effect that
A kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature of the present invention, can infuse in gel
Soluble silicon resin and catalyst are added in mold technique, direct in-situ reaction generates SiC nanowire in sintering；Organic siliconresin
Carbon and SiO are generated after cracking2, in the subsequent sintering process can in-situ preparation SiC nanowire, and then improve porous SiC power
Learn performance and absorbing property；The interconnected pore of the high-volume fractional formed after gel casting forming also promotes SiC nanowire
V-L-S growth, by adjusting sintering process, soluble silicon resin and catalyst content, i.e., changeable SiC nanowire is porous
Distribution and pattern in SiC ceramic, and then the absorbing property of controlled material, added soluble silicon resin is in low-temperature solid
The intensity that ceramic green can be greatly improved after change, facilitates its following process.
Detailed description of the invention
The present invention will be further described in detail with specific implementation method with reference to the accompanying drawing.
Fig. 1 is SiC nanowire of the invention/SiC porous ceramics microstructure schematic diagram one；
Fig. 2 is SiC nanowire of the invention/SiC porous ceramics microstructure schematic diagram two；
Fig. 3 is SiC nanowire of the invention/SiC porous ceramics absorbing property schematic diagram.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Specific embodiment 1:
Illustrate present embodiment, a kind of SiC nanowire/SiC porous ceramics for inhaling wave for high temperature below with reference to Fig. 1-3
Soluble silicon resin and catalyst is added during preparing ceramic green using gel injection-moulding method, in sintering in preparation method
Reaction in-situ generates SiC nanowire.
The preparation method the following steps are included:
Step 1: SiC powder and sintering aid ball milling mixing 12~for 24 hours, ball-milling medium is ethyl alcohol, mistake after ball milling drying
100~200 meshes；It is preferred that SiC powder and sintering aid ball milling mixing 12h are crossed 200 meshes, ball-milling medium is second after drying
The mass ratio of alcohol, sintering aid and SiC are 1:97, and sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Quality
Than for 1:0.6；Or preferably by SiC powder and sintering aid ball milling mixing for 24 hours, 200 meshes are crossed after drying, ball-milling medium is second
The mass ratio of alcohol, sintering aid and SiC are 1:99, and sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Quality
Than for 1:0.8.
Step 2: solvent, ceramic powder, dispersing agent, monomer, crosslinking agent, soluble silicon resin and catalyst ball milling are mixed
Conjunction 12~form slurry for 24 hours, it is polyvinylpyrrolidone that wherein solvent, which is alcohols, the dispersing agents such as ethyl alcohol, isopropanol and the tert-butyl alcohol,
Monomer is acrylamide, crosslinking agent N, N- methylene-bisacrylamide, and the soluble silicon resin is to dissolve in ethyl alcohol, different
The alcohols solvents such as propyl alcohol and the tert-butyl alcohol, the catalyst are ferrocene, FeCl3、Fe(NO3)3With Ni (NO3)2Equal metallic salts；
Soluble silicon resin content can control the quantity of SiC nanowire inside porous SiC ceramics, solubility in sample as shown in Figure 2
Silicone resin content and catalyst content are higher, therefore the SiC nanowire generated is also more.Sample sintering temperature shown in FIG. 1 is more
Height, and heating rate is faster, can arrive more straight SiC nanowire, and the sample in Fig. 2 is since sintering temperature is lower, heating rate
Relatively slow, what is obtained is curved SiC nanowire.SiC nanowire content is more, and the absorbing property of material is better.Contain straight SiC
The material mechanical performance of nano wire is more preferable, and absorbing property is slightly lower.
Step 3: mixed slurry being placed in vacuum and stirs de-bubble 10min, then initiator is added in the slurry and urges
Agent stirs injection molding after 10min, and is heated to 50~60 DEG C of heat preservation 0.5~2h gels；It is solidifying to be preferably heated to 60 DEG C of heat preservation 2h
Glue, wherein initiator is ammonium persulfate, and the mass ratio of initiator and monomer is 1:3, and catalyst is tetramethylethylenediamine, catalyst
Mass ratio with monomer is 1:30；Or 50 DEG C of heat preservation 2h gels are heated to, wherein initiator is ammonium persulfate, initiator and list
The mass ratio of body is 1:3, and catalyst is tetramethylethylenediamine, and the mass ratio of catalyst and monomer is 1:30.
Step 4: in the drying in 50~60 DEG C of baking oven after green body demoulding, 200 DEG C of heat preservations are heated to after being completely dried
2h makes the silicone resin crosslinking curing in green body；
Step 5: green body is placed in dumping in pyrolysis furnace；
Step 6: the green body after cracking dumping is placed in air pressure furnace and is sintered.
The sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio be 1:0.6~0.8；It is preferred that
SiC powder and sintering aid ball milling mixing 12h, Y2O3And Al2O3Mass ratio be 1:0.6 or SiC powder and sintering aid
Ball milling mixing for 24 hours, Y2O3And Al2O3Mass ratio be 1:0.8.
The volume ratio of the ceramic powder and solvent is 1:1.5~9, the mass ratio of dispersing agent and ceramic powder be 1:49~
124, the mass ratio of monomer and ceramic powder is 1:6~33, and the mass ratio of crosslinking agent and monomer is 1:20~30, soluble silicon tree
The mass ratio of rouge and ceramic powder is 1:19~99, and the mass ratio of catalyst and solvent is 1:97~99.9；Preferably ceramic powder
It is 1:9 with the volume ratio of ethyl alcohol, the mass ratio of polyvinylpyrrolidone and ceramic powder is 1:49, the matter of monomer and ceramic powder
For amount than being 1:6, the mass ratio of crosslinking agent and monomer is 1:30, and the mass ratio of soluble silicon resin and ceramic powder is 1:19, is urged
The mass ratio of agent and solvent is 1:97；Or the volume ratio of ceramic powder and ethyl alcohol is 1:1.5, polyvinylpyrrolidone and pottery
The mass ratio of porcelain powder is 1:124, and the mass ratio of monomer and ceramic powder is 1:6, and the mass ratio of crosslinking agent and monomer is 1:30,
The mass ratio of soluble silicon resin and ceramic powder is 1:99, and the mass ratio of catalyst and solvent is 1:99.
The initiator being added in the slurry is ammonium persulfate, and the catalyst being added in slurry is tetramethylethylenediamine.
The mass ratio of the initiator and monomer is 1:3~10, and the mass ratio of catalyst and monomer is 1:30~200.
The dump temperature be 550~650 DEG C, heating rate be 0.3 DEG C/min, soaking time 2h, atmosphere be nitrogen or
Argon gas；It is preferred that green body is placed in dumping in pyrolysis furnace, dump temperature is 650 DEG C, and heating rate is 0.3 DEG C/min, soaking time
2h, atmosphere are argon gas；Or green body is placed in dumping in pyrolysis furnace, dump temperature is 550 DEG C, and heating rate is 0.5 DEG C/min,
Soaking time 1h, atmosphere are argon gas.
The step of sintering is first to be warming up to 1500 DEG C of 0.5~1h of heat preservation with 10 DEG C/min, then be warming up to 5 DEG C/min
1700~1900 DEG C of 1~4h of heat preservation；It is sintered it is preferred that the green body after cracking is placed in air pressure furnace, is first warming up to 10 DEG C/min
1500 DEG C of heat preservation 0.5h, then 1800 DEG C of heat preservation 2h are warming up to 5 DEG C/min, sintering atmosphere is argon gas, pressure 0.4MPa；Or
Green body after cracking is placed in air pressure furnace and is sintered, 1500 DEG C of heat preservation 1h are first warming up to 10 DEG C/min, then with 5 DEG C/min heating
To 1900 DEG C of heat preservation 2h, sintering atmosphere is argon gas, pressure 0.4MPa, and the sintering atmosphere is argon gas, pressure is 0.4~
1MPa。
The mass ratio of the SiC powder and sintering aid is 1:89~99；It is preferred that the mass ratio of sintering aid and SiC are 1:
97 or the mass ratio of sintering aid and SiC be 1:99.
Specific embodiment 2:
Illustrate present embodiment, a kind of SiC nanowire/SiC porous ceramics for inhaling wave for high temperature below with reference to Fig. 1-3
Soluble silicon resin and catalyst is added during preparing ceramic green using gel injection-moulding method, in sintering in preparation method
Reaction in-situ generate SiC nanowire, the preparation method the following steps are included:
Step 1: by SiC powder and sintering aid ball milling mixing 12h, crossing 200 meshes after drying, ball-milling medium is ethyl alcohol,
The mass ratio of sintering aid and SiC are 1:97, and sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio
For 1:0.6.
Step 2: by ethyl alcohol, ceramic powder, polyvinylpyrrolidone, monomer, crosslinking agent, soluble silicon resin and FeCl3
Ball milling mixing 12h, monomer are acrylamide, crosslinking agent N, N- methylene-bisacrylamide, the volume of ceramic powder and ethyl alcohol
Than for 1:9, N, the mass ratio of N- methylene-bisacrylamide and ceramic powder is 1:49, and the mass ratio of monomer and ceramic powder is
The mass ratio of 1:6, crosslinking agent and monomer is 1:30, and the mass ratio of soluble silicon resin and ceramic powder is 1:19, catalyst with
The mass ratio of solvent is 1:97.
Step 3: mixed slurry being placed in vacuum and stirs de-bubble 10min, then initiator is added in the slurry and urges
Agent stirs injection molding after 10min, and is heated to 60 DEG C of heat preservation 2h gels, and wherein initiator is ammonium persulfate, initiator and monomer
Mass ratio be 1:3, catalyst is tetramethylethylenediamine, and the mass ratio of catalyst and monomer is 1:30.
Step 4: in the drying in 50 DEG C of baking oven after green body demoulding, 200 DEG C of heat preservation 2h are heated to after being completely dried to be made
Silicone resin crosslinking curing in green body.
Step 5: being placed in dumping in pyrolysis furnace for green body, and dump temperature is 550 DEG C, and heating rate is 0.5 DEG C/min, is protected
Warm time 1h, atmosphere are argon gas.
Step 6: the green body after cracking being placed in air pressure furnace and is sintered, and is first warming up to 1500 DEG C of heat preservations with 10 DEG C/min
0.5h, then 1800 DEG C of heat preservation 2h are warming up to 5 DEG C/min, sintering atmosphere is argon gas, pressure 0.4MPa.
Specific embodiment 3:
Illustrate present embodiment, a kind of SiC nanowire/SiC porous ceramics for inhaling wave for high temperature below with reference to Fig. 1-3
Soluble silicon resin and catalyst is added during preparing ceramic green using gel injection-moulding method, in sintering in preparation method
Reaction in-situ generate SiC nanowire, the preparation method the following steps are included:
Step 1: for 24 hours by SiC powder and sintering aid ball milling mixing, crossing 200 meshes after drying, ball-milling medium is ethyl alcohol,
The mass ratio of sintering aid and SiC are 1:99, and sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio
For 1:0.8.
Step 2: by ethyl alcohol, ceramic powder, polyvinylpyrrolidone, monomer, crosslinking agent, soluble silicon resin and two cyclopentadienyls
For 24 hours, body is acrylamide to iron ball milling mixing, and the volume ratio of ceramic powder and ethyl alcohol is 1:1.5, polyvinylpyrrolidone and ceramics
The mass ratio of powder is 1:124, and the mass ratio of monomer and ceramic powder is 1:6, and the mass ratio of crosslinking agent and monomer is 1:30, can
The mass ratio of dissolubility silicone resin and ceramic powder is 1:99, and the mass ratio of catalyst and solvent is 1:99；
Step 3: mixed slurry being placed in vacuum and stirs de-bubble 10min, then initiator is added in the slurry and urges
Agent stirs injection molding after 10min, and is heated to 50 DEG C of heat preservation 2h gels, and wherein initiator is ammonium persulfate, initiator and monomer
Mass ratio be 1:3, catalyst is tetramethylethylenediamine, and the mass ratio of catalyst and monomer is 1:30.
Step 4: in the drying in 50 DEG C of baking oven after green body demoulding, 200 DEG C of heat preservation 2h are heated to after being completely dried to be made
Silicone resin crosslinking curing in green body.
Step 5: being placed in dumping in pyrolysis furnace for green body, and dump temperature is 650 DEG C, and heating rate is 0.3 DEG C/min, is protected
Warm time 2h, atmosphere are argon gas.
Step 6: the green body after cracking being placed in air pressure furnace and is sintered, and is first warming up to 1500 DEG C of heat preservation 1h with 10 DEG C/min,
1900 DEG C of heat preservation 2h are warming up to 5 DEG C/min again, sintering atmosphere is argon gas, pressure 0.4MPa.
Certainly, above description is not limitation of the present invention, and the present invention is also not limited to the example above, the art
The variations, modifications, additions or substitutions that those of ordinary skill is made within the essential scope of the present invention also belong to guarantor of the invention
Protect range.
Claims (10)
1. a kind of SiC nanowire/SiC porous ceramics preparation method for inhaling wave for high temperature, it is characterised in that: infused using gel
Soluble silicon resin and catalyst is added during preparing ceramic green in modulus method, and in sintering, reaction in-situ generates SiC nanometers
Line.
2. a kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature according to claim 1,
Be characterized in that: the preparation method the following steps are included:
Step 1: SiC powder and sintering aid ball milling mixing 12~for 24 hours, ball-milling medium is ethyl alcohol, cross 100 after ball milling drying~
200 meshes；
Step 2: by solvent, ceramic powder, dispersing agent, monomer, crosslinking agent, soluble silicon resin and catalyst ball milling mixing 12
~slurry is formed for 24 hours；
Step 3: mixed slurry being placed in vacuum and stirs de-bubble 10min, then initiator and catalysis are added in the slurry
Agent stirs injection molding after 10min, and is heated to 50~60 DEG C of heat preservation 0.5~2h gels；
Step 4: in the drying in 50~60 DEG C of baking oven after green body demoulding, 200 DEG C of heat preservation 2h are heated to after being completely dried to be made
Silicone resin crosslinking curing in green body；
Step 5: green body is placed in dumping in pyrolysis furnace；
Step 6: the green body after cracking dumping is placed in air pressure furnace and is sintered.
3. a kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature according to claim 2,
Be characterized in that: the volume ratio of the ceramic powder and solvent is 1:1.5~9, and the mass ratio of dispersing agent and ceramic powder is 1:49
~124, the mass ratio of monomer and ceramic powder is 1:6~33, and the mass ratio of crosslinking agent and monomer is 1:20~30, soluble silicon
The mass ratio of resin and ceramic powder is 1:19~99, and the mass ratio of catalyst and solvent is 1:97~99.9.
4. a kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature according to claim 3,
Be characterized in that: the solvent is ethyl alcohol, isopropanol and the tert-butyl alcohol, and dispersing agent is polyvinylpyrrolidone, and monomer is acrylamide,
Crosslinking agent is N, and N- methylene-bisacrylamide, the soluble silicon resin is to dissolve in ethyl alcohol, isopropanol and the tert-butyl alcohol, institute
The catalyst stated is ferrocene, FeCl3、Fe(NO3)3With Ni (NO3)2。
5. a kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature according to claim 2,
Be characterized in that: the sintering aid is by Y2O3And Al2O3Powder composition, Y2O3And Al2O3Mass ratio be 1:0.6~0.8.
6. a kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature according to claim 2,
Be characterized in that: the initiator being added in the slurry is ammonium persulfate, and the catalyst being added in slurry is tetramethylethylenediamine.
7. a kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature according to claim 6,
Be characterized in that: the mass ratio of the initiator and monomer is 1:3~10, and the mass ratio of catalyst and monomer is 1:30~200.
8. a kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature according to claim 2,
Be characterized in that: the dump temperature be 550~650 DEG C, heating rate be 0.3 DEG C/min, soaking time 2h, atmosphere be nitrogen or
Argon gas.
9. a kind of SiC nanowire/SiC porous ceramics preparation method that wave is inhaled for high temperature according to claim 2,
It is characterized in that: to be first warming up to 1500 DEG C of 0.5~1h of heat preservation with 10 DEG C/min the step of the sintering, then being heated up with 5 DEG C/min
To 1700~1900 DEG C of 1~4h of heat preservation, the sintering atmosphere is argon gas, and pressure is 0.4~1MPa.
10. a kind of SiC nanowire/SiC porous ceramics for inhaling wave for high temperature according to any one of claims 1 to 9
Preparation method, it is characterised in that: the mass ratio of the SiC powder and sintering aid is 1:89~99.
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