CN103724046B - A kind of SiC foam and preparation method thereof - Google Patents
A kind of SiC foam and preparation method thereof Download PDFInfo
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- CN103724046B CN103724046B CN201310412069.0A CN201310412069A CN103724046B CN 103724046 B CN103724046 B CN 103724046B CN 201310412069 A CN201310412069 A CN 201310412069A CN 103724046 B CN103724046 B CN 103724046B
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Abstract
A kind of SiC foam and preparation method thereof.This foam is made up of the SiC coating of carbon foam substrate and the SiC film and foam surface that are attached to foam hole inwall, and present the structure of sandwich, the porosity of core foam is 70% ~ 95%, and aperture is between 200 ~ 2000 μm.Described SiC film is evenly attached to the hole inwall of open cell carbon foam, and thickness is 50nm ~ 2 μm.SiC coating is combined in foam surface, and thickness is 5 ~ 100 μm, can be fine and close, also can be loose.A preparation method for SiC foam, is characterized in that the step comprising following order: (1), by polyurethane foam pyrolysis, makes carbon foam; (2) SiC film is prepared; (3) preparation of surperficial SiC coating; (4) deposition terminates rear cooling taking-up, namely obtains a kind of SiC foam.
Description
Technical field
The present invention relates to a kind of foam and preparation method thereof, particularly relate to a kind of SiC foam and preparation method thereof.
Background technology
The charcoal base foam materials being representative with Carbon foam and sic foam has important application background with its distinctive lightweight, high strength, high temperature resistant and corrosion resistant feature in Aeronautics and Astronautics, naval vessel and national defence.The sixties in last century can be traced back to the research of charcoal base foam materials, main employing fluoropolymer resin is starting material, obtain through foaming and charing, prepared Carbon foam material fragility is comparatively large, is research and develop as adiabatic filling material for a long time always.
Publication number is that the Chinese invention patent of 102101785A relates to foamed ceramics field, and specifically a kind of not only had macro-scale three-dimensional communication aperture but also two dimension foams potteries with micron order three-dimensional communication aperture and preparation method thereof.Foam silicon carbide ceramics has three-dimensional networks structure; Macroscopically show as grade aperture; Ceramic skeleton muscle inside shows as the mesh that micron order is interconnected.The present invention is in the process of foamed ceramics blank forming, evenly pore-forming material is mixed in silicon carbide slurry, make foam silicon carbide ceramics be prepared into two dimension foam pottery, two yardstick foam silicon carbide ceramics is a kind of three-dimensional networks foamed ceramics simultaneously with macroscopical mm-scale aperture and the inner micro-meter scale aperture of skeleton muscle.As the reinforcement of ceramic/metallic double continuous phase composite material, two yardstick silicon carbide foam ceramic material can be eliminated foam framework crackle in matrix material, improves composite quality, expand the application of matrix material in friction catch, armor facing and Electronic Packaging etc.
Publication number is that the Chinese invention patent of 103011887A discloses a kind of foam silicon carbide ceramics, calculates by weight, and its material comprises 80 ~ 95 parts of silicon carbide micro-powder particles, 5 ~ 20 parts of Polycarbosilane powder, 40 ~ 170 parts of organic solvents; Its template is polyurethane sponge.The present invention utilizes Polycarbosilane to dissolve in the feature of organic solvent, organic solvent pulps is made in it and ceramic powder, adopt powder sintered ratio juris, polyurethane foam is utilized to flood organic solvent pulps, and by thermal oxidative treatment to improve poly carbon silane ceramics productive rate, and then sintering prepares foam silicon carbide ceramics under an inert atmosphere, this preparation method has the advantage that sintering temperature is low, efficiency is high, product purity is high, efficiently avoid Conventional silicon carbide foamed ceramics complicated process of preparation, introduces the difficult problem that impurity is many, sintering temperature is high.
Perforated foams is a kind of Multifunction material, there is three-dimensional net structure, porosity is high, specific surface area is large, physical strength is high and the excellent feature of antioxidant property, be the desirable equivalent material of fragility porous ceramics, have broad application prospects in fields such as various high-temperature catalytic carrier, anti-corrosion catalyst carrier, strainer and heat exchangers.
Summary of the invention
The present invention aims to provide a kind of SiC foam and preparation method thereof.This SiC foam has sandwich structure, is made up of the SiC coating of carbon foam substrate and the SiC film and foam surface that are attached to foam hole inwall.Thermal conductivity due to carbon foam is the thermal conductivity of 150W/mk, SiC is 120W/mk, and both thermal expansions are close, and SiC can be attached on carbon foam base plate well, effectively improves intensity and the antioxidant property of carbon foam.
Described carbon foam substrate is a kind of foam of open-celled structure, and inside presents tridimensional network, is cross-linked and forms, have large surface-area, can fill the many kinds of substance of solid, liquid, gas state by irregular holes not of uniform size.
Described SiC film is evenly attached to the hole inwall of open cell carbon foam, and thickness is 50nm ~ 2 μm.
Described SiC coating is combined in foam surface, and thickness is 5 ~ 100 μm, and upper layer can be fine and close, also can be the short texture that there is hole.
Above-mentioned SiC foam has sandwich structure, and the porosity of core is 70% ~ 95%, and aperture is between 200 ~ 2000 μm.
A preparation method for SiC foam, is characterized in that the step comprising following order:
(1) by polyurethane foam pyrolysis, carbon foam is made;
(2) SiC film is prepared: obtained carbon foam is put into CVI stove, passes into CH
3siCl
3and H
2, control temperature and time, adhere to certain thickness SiC film at the perforate inwall of carbon foam;
(3) preparation of surperficial SiC coating: take out foam silicon from CVI stove, put into CVD stove: with trichloromethyl silane (CH
3siCl
3, MTS) and be precursor raw material, H
2make carrier gas and diluent gas, adopting mass flow controller to control gas flow is 60 ~ 120mL/min, and by Bubbling method, MTS is brought into reaction chamber, depositing temperature is 1050 ~ 1200 DEG C, and pressure is normal pressure, and the time is 40 ~ 100h;
(4) deposition terminates rear cooling taking-up, namely obtains a kind of SiC foam.
According to above-mentioned preparation method, carbon foam is obtained by polyurethane foam heating carbonization, and concrete technological process is carried out in two steps: first in atmosphere, polyurethane foam heated at 200 ~ 255 DEG C; Then in an inert atmosphere, carbonization at 700 ~ 900 DEG C.
Major advantage of the present invention is: 1. obtained SiC foam quality is light, anti-oxidant, has higher toughness and rigidity, specific inductivity is high, specific surface area is large, chemical resistance is excellent, can use for a long time under rugged environment; 2. the preparation of foamy structure does not need complicated technology and equipment, reduces costs; 3. the foamy structure of perforate can fill several functions material, effectively improves speed of reaction and effect; 4. adopt the preparation method of CVI, CVD, film is even, is combined closely with matrix.
Accompanying drawing explanation
Be illustrated as a kind of schematic diagram of SiC foam.
Diagram 10 is surperficial SiC coating; 20 for being attached with the carbon foam of SiC film.
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) pyrolysis of polyurethane foam: first in atmosphere, at 255 DEG C, polyurethane foam is heated; Then, in nitrogen atmosphere, carbonization at 900 DEG C, namely obtains carbon foam;
(2) SiC film is prepared: obtained carbon foam is put into CVI stove, passes into CH
3siCl
3and H
2, control temperature and time, at the Si film of the perforate inwall attachment 50nm thickness of carbon foam;
(3) preparation of surperficial SiC coating: take out foam silicon from CVI stove, put into CVD stove: with trichloromethyl silane (CH
3siCl
3, MTS) and be precursor raw material, H
2make carrier gas and diluent gas, adopting mass flow controller to control gas flow is 60mL/min, and by Bubbling method, MTS is brought into reaction chamber, depositing temperature is 1050 DEG C, and pressure is normal pressure, and the time is 40h;
(4) deposition terminates rear cooling taking-up, namely obtains a kind of SiC foam.
The obtained SiC foam of aforesaid method has sandwich structure, is made up of the SiC coating of carbon foam substrate and the SiC film and foam surface that are attached to foam hole inwall.The porosity of core foam is 85%, and aperture is 1000 μm, and the thickness of surperficial SiC coating is 10 μm.This froth quality is light, anti-oxidant, has higher toughness and rigidity, specific inductivity is high, specific surface area is large, chemical resistance is excellent, can use for a long time under rugged environment.
Embodiment 2
(1) pyrolysis of polyurethane foam: first in atmosphere, at 240 DEG C, polyurethane foam is heated; Then, in argon gas atmosphere, carbonization at 850 DEG C, namely obtains carbon foam;
(2) SiC film is prepared: obtained carbon foam is put into CVI stove, passes into CH
3siCl
3and H
2, control temperature and time, at the Si film of the perforate inwall attachment 100nm thickness of carbon foam;
(3) preparation of surperficial SiC coating: take out foam silicon from CVI stove, put into CVD stove: with trichloromethyl silane (CH
3siCl
3, MTS) and be precursor raw material, H
2make carrier gas and diluent gas, adopting mass flow controller to control gas flow is 100mL/min, and by Bubbling method, MTS is brought into reaction chamber, depositing temperature is 1100 DEG C, and pressure is normal pressure, and the time is 60h;
(4) deposition terminates rear cooling taking-up, namely obtains a kind of SiC foam.
The obtained SiC foam of aforesaid method has sandwich structure, is made up of the SiC coating of carbon foam substrate and the SiC film and foam surface that are attached to foam hole inwall.The porosity of core foam is 70%, and aperture is 500 μm, and the thickness of surperficial SiC coating is 30 μm.This froth quality is light, anti-oxidant, has higher toughness and rigidity, specific inductivity is high, specific surface area is large, chemical resistance is excellent, can use for a long time under rugged environment.
Above are only the present invention's two embodiments, 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 SiC foam, be made up of the SiC coating of carbon foam substrate and the SiC film and foam surface that are attached to foam hole inwall, present the structure of sandwich, it is characterized in that described carbon foam substrate is a kind of foam of open-celled structure, porosity is 70% ~ 95%, and aperture is between 210 ~ 2000 μm, and inside presents tridimensional network, there is large surface-area, the many kinds of substance of solid, liquid, gas state can be filled; Described SiC film is evenly attached to the hole inwall of open cell carbon foam, and thickness is 50nm ~ 2 μm; Described SiC coating is combined in foam surface, and thickness is 5 ~ 100 μm.
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CN104201317B (en) * | 2014-09-10 | 2017-01-18 | 太仓派欧技术咨询服务有限公司 | Preparation method of heat insulating carbon foam separator of lead-acid cell |
CN106904973B (en) * | 2017-02-22 | 2020-07-24 | 南京航空航天大学 | Light high-strength foam carbon-based heat-insulating composite material |
CN109836165B (en) * | 2017-11-27 | 2021-10-15 | 航天特种材料及工艺技术研究所 | SiC foam and preparation method thereof |
CN108751159A (en) * | 2018-05-27 | 2018-11-06 | 南京航空航天大学 | A kind of compound carbon foam of CVI-SiC nano wires enhancing |
CN109020469A (en) * | 2018-08-17 | 2018-12-18 | 苏州宏久航空防热材料科技有限公司 | A kind of SiO2Aeroge/SiC foam composite insulation material and preparation method thereof |
CN110066175B (en) * | 2019-05-13 | 2020-10-27 | 中南大学 | Preparation method of ultralight carbide ceramic foam |
Citations (2)
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CN1719287A (en) * | 2005-06-29 | 2006-01-11 | 中国人民解放军国防科学技术大学 | Sandwiched type structure SIC base composite material light reflection mirrow and its preparation method |
CN101336206A (en) * | 2005-12-29 | 2008-12-31 | 格拉弗技术国际控股有限公司 | Glassy carbon coated carbon foam |
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CN1719287A (en) * | 2005-06-29 | 2006-01-11 | 中国人民解放军国防科学技术大学 | Sandwiched type structure SIC base composite material light reflection mirrow and its preparation method |
CN101336206A (en) * | 2005-12-29 | 2008-12-31 | 格拉弗技术国际控股有限公司 | Glassy carbon coated carbon foam |
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