CN100395211C - Method for preparing porous silicon carbide ceramic with high porosity - Google Patents
Method for preparing porous silicon carbide ceramic with high porosity Download PDFInfo
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Abstract
The present invention relates to a preparation method of porous silicon carbide ceramics with high porosity, which belongs to the field of the preparation process of ceramic materials. In the method, silicon powder, phenolic resin and alcohol with certain mass ratio are prepared into coat-mix powder by the coat-mix process, then the coat-mix powder is treated by low-temperature low-pressure forming to be prepared into ceramic compacts, the ceramic compacts are carbonized at a high temperature, and finally, the carbonized samples are sintered at a high temperature to obtain porous silicon carbide ceramics with the porosity of higher than 80%. The method has the advantages of simple process, high production efficiency, energy conservation and good environment compatibility, and is a method which can prepare porous silicon carbide ceramics with high porosity.
Description
Technical field
The invention belongs to ceramic materials preparation technology field, particularly a kind of preparation method of high porosity silicon carbide ceramics.
Technical background
Because it is good to have perviousness, specific surface area is big, density is low, the intensity height, thermal conductivity is little, high temperature resistant, wear-resistant, chemical stability is good, premium propertiess such as good radioprotective and electromagnetic consumable, the porous silicon carbide material has been widely used in aerospace, the energy, machinery, metallurgical, chemical industry, environmental protection, military project, a plurality of ambits such as electronics and biology, relating to fluid separation filters, diffusion, heat insulation, sound-absorbing, sensing, the purposes of all many-sides such as electrochemical process and catalytic reaction engineering, can make strainer, separation and support of the catalyst etc., therefore the research of porous silicon carbide material has caused the great attention of global material educational circles, new preparation method arises at the historic moment, and the preparation system also constantly improves.
The preparation of porous silicon carbide also has bibliographical information, and (application number: 03116370.X) reported a kind of is pore-forming material with the yeast powder to Chinese patent, and SiC is an aggregate, Al
2O
3, Suzhou soil and wilkinite be the preparation method of the carborundum porous ceramics of sintering aid.This method gained carborundum porous ceramics pore size distribution is more even, easily control.But this method resulting product porosity lower (45~60%), complex forming technology, product purity is low.Zhu Xinwen etc. have reported another preparation method at " Mater Sci Eng, 2002, A323:232-238 ", and promptly adopting has silicon carbide micro-powder, α-Al
2O
3, carboxymethyl cellulose, clay and silicon sol preparation mud dipping organic foam, success develop the silicon carbide screen like and porous ceramic that can be used for filtering molten metal and handle high-temperature flue gas.This method technology is simple, easy to operate, and is not high to equipment requirements, with low cost, is suitable for industrialization, but can not prepare the small-bore goods of high purity, complex-shaped, composition controllable density.In addition, the eliminating of organic foam also can cause environmental pollution problems in preparation process." J Eur Ceram Soc; 1998; 18 (14): 1961-1973 " report has at first obtained preform with natural timber carbonizing treatment in inert atmosphere of different apertures and composition, then liquid-state silicon is injected wherein, made silicon and carbon prepared in reaction go out to inherit the porous silicon carbide material of natural timber structure.These method raw material sources extensively, good economy performance, easily processing, easy mass production, and Environmental compatibility is good, but the aperture size of this method gained porous silicon carbide material and void content distribute and be subjected to the control of initial wood materials structure and performance.French Patent (application number: 87-14742) reported a kind of method that adopts high-ratio surface activated carbon and the reaction of gas phase silicon monoxide to generate porous silicon carbide, but the carbofrax material pore size distribution range of this method preparation is wide.Patent WO 03/024892 A1 has also reported a kind of method of porous silicon carbide ceramic, and the main raw material of this method comprises: SiC powder (main raw material), SiO
2Powder or Si powder (silicon source), carbon black or Graphite Powder 99 (carbon source) and at least a organism (binding agent).These raw materials are made behind the base mud by having made porous silicon carbide ceramic after the operations such as moulding, drying, cracking and high temperature sintering, performances such as its aperture, porosity can be controlled by changing proportioning raw materials and processing condition, but this method temperature of reaction very high (2200~2600 ℃).It is silicon source and carbon source with silica flour and carbon dust respectively that U.S. Pat 005248462A has also introduced a kind of, shot or other sphere materials are the continuous preparation technology that pore-forming material prepares the foam silicon carbon material, this technology (evenly wraps in the mixture of silica flour, carbon dust and binding agent on the shot by moulding, and fill up hole between the shot), heating (remove low-melting shot and form the hole) and three steps of high temperature sintering (making the reaction of silicon and carbon generate) generate the foam silicon carbon material, still the aperture of this method gained porous silicon carbide material is bigger.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of porous silicon carbide ceramic with high porosity, described method is a raw material with silica flour (silicon source), resol (binding agent) and alcohol, after the mixed technology of bag, low-temp low-pressure moulding, high temperature cabonization processing and four step process of high temperature sintering, obtain the porous silicon carbide ceramic with high porosity material, it is characterized in that: concrete processing step is:
1) by the mass ratio 1 of silica flour, resol and alcohol: (0.25~1.1): 2 are mixed into slurry;
2) preparation coat mix powder: mixed slurry is heat-treated at 30~80 ℃, and stir 30~120min; Be cooled to then below 10 ℃, 10~60min is stirred in deepfreeze in 0~10 ℃ of scope simultaneously again; Mixed slurry is injected in the entry injection pressure 0.2~1.2MPa; And carry out burin-in process, churning time 30~120min at 30~90 ℃; The vacuum-drying temperature is 40~100 ℃, and be 30~120min time of drying, obtains the powder that the resol bag mixes silica flour;
3) powder that the resol bag is mixed silica flour is at the low-temp low-pressure molding ceramic green: 60~100 ℃ of mold temperatures; Forming pressure 0.05~0.2MPa; Soaking time 30~120min obtains ceramic green;
4) carbonizing treatment of ceramic green: 600~1000 ℃ of carbonization temperatures; 0.3~1 ℃/min of temperature rise rate; Argon flow amount 50~200ml/min carries out carbonization to ceramic green under soaking time 1~4h;
5) high temperature sintering is handled: with the ceramic green of carbonizing treatment 1300~1800 ℃ of sintering temperatures; Temperature rise rate 1-5 ℃/min; At flow is the argon shield of 50~200ml/min or under vacuum condition; Soaking time 1~8 hour finally obtains the porous silicon carbide ceramic with high porosity material.
2124 resol of 2120 resol that described resol as binding agent is Xinhua Resin Factory, Shanghai, 214 resol, Changchun chemical industry two factories, 401 resol and 407 resol of Tianjin resin processing plant, Suzhou resin processing plant and the ammonia resol of Beijing 251 factories and in the ba phenolic resin any one.
Beneficial effect of the present invention is bag to be mixed technology, low-temp low-pressure moulding, high temperature cabonization processing and high-sintering process combine, and utilizes silica flour and resol to prepare the porous silicon carbide ceramic with high porosity material.Therefore, this law can reduce cost greatly and process implementing carries out the transition to production in enormous quantities simply, easily, be a kind ofly can prepare high strength, high porosity (greater than 80%), mean pore size is in the method for the porous silicon carbide ceramic of 100~300 μ m and even aperture distribution.
Embodiment
The invention provides a kind of preparation method of porous silicon carbide ceramic with high porosity, described method is a raw material with silica flour (silicon source), resol (binding agent) and alcohol, after the mixed technology of bag, low-temp low-pressure moulding, high temperature cabonization processing and four step process of high temperature sintering, obtain the porous silicon carbide ceramic with high porosity material, it is characterized in that: concrete processing step is:
1) by the mass ratio 1 of silica flour, resol and alcohol: (0.25~1.1): 2 are mixed into slurry;
2) preparation coat mix powder: mixed slurry is heat-treated at 30~80 ℃, and stir 30~120min; Be cooled to then below 10 ℃, 10~60min is stirred in deepfreeze in 0~10 ℃ of scope simultaneously again; Mixed slurry is injected in the entry injection pressure 0.2~1.2MPa; And carry out burin-in process, churning time 30~120min at 30~90 ℃; The vacuum-drying temperature is 40~100 ℃, and be 30~120min time of drying, obtains the powder that the resol bag mixes silica flour;
3) powder that the resol bag is mixed silica flour is at the low-temp low-pressure molding ceramic green: 60~100 ℃ of mold temperatures; Forming pressure 0.05~0.2MPa; Soaking time 30~120min obtains ceramic green;
4) carbonizing treatment of ceramic green: 600~1000 ℃ of carbonization temperatures; 0.3~1 ℃/min of temperature rise rate; Argon flow amount 50~200ml/min carries out carbonization to ceramic green under soaking time 1~4h;
5) high temperature sintering is handled: with the ceramic green of carbonizing treatment 1300~1800 ℃ of sintering temperatures; Temperature rise rate 1-5 ℃/min; At flow is the argon shield of 50~200ml/min or under vacuum condition; Soaking time 1~8 hour finally obtains the porous silicon carbide ceramic with high porosity material.
2124 resol of 2120 resol that described resol as binding agent is Xinhua Resin Factory, Shanghai, 214 resol, Changchun chemical industry two factories, 401 resol and 407 resol of Tianjin resin processing plant, Suzhou resin processing plant and the ammonia resol of Beijing 251 factories and in the ba phenolic resin any one.
The present invention be listed below embodiment in order better to explain:
Embodiment 1
At first adopt bag to mix technology silica flour, ba phenolic resin are mixed with alcohol (mass ratio 1: 0.25: 2), at 30 ℃ of thermal treatment 120min, at 0 ℃ of deepfreeze 10min, injection pressure 0.2MPa, at 30 ℃ of burin-in process 120min,, obtain coat mix powder at 40 ℃ of vacuum-drying 120min; Then with coat mix powder at 60 ℃, 0.05MPa pressure down insulation 120min moulding obtains ceramic green; Then ceramic green (50ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 600 ℃, 0.3 ℃/min of temperature rise rate, insulation 240min; The powder (50ml/min) under argon shield that carbonizing treatment is obtained carries out high temperature sintering at last, and temperature is 1300 ℃, and 1 ℃/min of temperature rise rate is incubated 8 hours and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 2
At first adopt bag to mix technology silica flour, ba phenolic resin are mixed with alcohol (mass ratio 1: 0.25: 2), at 30 ℃ of thermal treatment 120min, at 0 ℃ of deepfreeze 10min, injection pressure 0.2MPa, at 30 ℃ of burin-in process 120min,, obtain coat mix powder at 40 ℃ of vacuum-drying 120min; Then with coat mix powder at 80 ℃, 0.1MPa pressure down insulation 60min moulding obtains ceramic green; Then ceramic green (100ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 800 ℃, 0.5 ℃/min of temperature rise rate, insulation 120min; The powder (100ml/min) under argon shield that carbonizing treatment is obtained carries out high temperature sintering at last, and temperature is 1500 ℃, and 2.5 ℃/min of temperature rise rate is incubated 4 hours and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 3
At first adopt bag to mix technology silica flour, ba phenolic resin are mixed with alcohol (mass ratio 1: 0.5: 2), at 30 ℃ of thermal treatment 120min, at 0 ℃ of deepfreeze 10min, injection pressure 0.2MPa, at 30 ℃ of burin-in process 120min,, obtain coat mix powder at 40 ℃ of vacuum-drying 120min; Then with coat mix powder at 100 ℃, 0.2MPa pressure down insulation 30min moulding obtains ceramic green; Then ceramic green (200ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 1000 ℃, 1 ℃/min of temperature rise rate, insulation 60min; The powder (200ml/min) under argon shield that carbonizing treatment is obtained carries out high temperature sintering at last, and temperature is 1800 ℃, and 5 ℃/min of temperature rise rate is incubated 1 hour and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 4
At first adopt bag to mix technology silica flour, ba phenolic resin are mixed with alcohol (mass ratio 1: 0.8: 2), at 45 ℃ of thermal treatment 90min, at 5 ℃ of deepfreeze 30min, injection pressure 0.6MPa, at 60 ℃ of burin-in process 90min,, obtain coat mix powder at 60 ℃ of vacuum-drying 90min; Then with coat mix powder at 60 ℃, 0.05MPa pressure down insulation 120min moulding obtains ceramic green; Then ceramic green (100ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 800 ℃, 0.5 ℃/min of temperature rise rate, insulation 120min; The powder (200ml/min) under argon shield that carbonizing treatment is obtained carries out high temperature sintering at last, and temperature is 1800 ℃, and 5 ℃/min of temperature rise rate is incubated 1 hour and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 5
At first adopt bag to mix technology silica flour, ba phenolic resin are mixed with alcohol (mass ratio 1: 0.5: 2), at 45 ℃ of thermal treatment 90min, at 5 ℃ of deepfreeze 30min, injection pressure 0.6MPa, at 60 ℃ of burin-in process 90min,, obtain coat mix powder at 60 ℃ of vacuum-drying 90min; Then with coat mix powder at 80 ℃, 0.1MPa pressure down insulation 60min moulding obtains ceramic green; Then ceramic green (200ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 1000 ℃, 1 ℃/min of temperature rise rate, insulation 60min; At last the powder (50ml/min) under argon shield that carbonizing treatment obtained is carried out high temperature sintering, temperature is 1300 ℃, and 1 ℃/min of temperature rise rate is incubated 8 hours and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 6
At first adopt bag to mix technology silica flour, ba phenolic resin are mixed with alcohol (mass ratio 1: 0.5: 2), at 45 ℃ of thermal treatment 90min, at 5 ℃ of deepfreeze 30min, injection pressure 0.6MPa, at 60 ℃ of burin-in process 90min,, obtain coat mix powder at 60 ℃ of vacuum-drying 90min; Then with coat mix powder at 100 ℃, 0.2MPa pressure down insulation 30min moulding obtains ceramic green; Then ceramic green (50ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 600 ℃, 0.3 ℃/min of temperature rise rate, insulation 240min; At last the powder (100ml/min) under argon shield that carbonizing treatment obtained is carried out high temperature sintering, temperature is 1500 ℃, and 2.5 ℃/min of temperature rise rate is incubated 4 hours and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 7
At first adopt bag to mix technology silica flour, ba phenolic resin are mixed with alcohol (mass ratio 1: 1.1: 2), at 80 ℃ of thermal treatment 60min, at 10 ℃ of deepfreeze 60min, injection pressure 1.2MPa, at 90 ℃ of burin-in process 60min,, obtain coat mix powder at 100 ℃ of vacuum-drying 30min; Then with coat mix powder at 60 ℃, 0.05MPa pressure down insulation 120min moulding obtains ceramic green; Then ceramic green (200ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 1000 ℃, 1 ℃/min of temperature rise rate, insulation 60min; The powder (100ml/min) under argon shield that carbonizing treatment is obtained carries out high temperature sintering at last, and temperature is 1500 ℃, and 2.5 ℃/min of temperature rise rate is incubated 4 hours and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 8
At first adopt bag to mix technology silica flour, ba phenolic resin are mixed with alcohol (mass ratio 1: 1.1: 2), at 80 ℃ of thermal treatment 60min, at 10 ℃ of deepfreeze 60min, injection pressure 1.2MPa, at 90 ℃ of burin-in process 60min,, obtain coat mix powder at 100 ℃ of vacuum-drying 30min; Then with coat mix powder at 80 ℃, 0.1MPa pressure down insulation 60min moulding obtains ceramic green; Then ceramic green (50ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 600 ℃, 0.3 ℃/min of temperature rise rate, insulation 240min; The powder (200ml/min) under argon shield that carbonizing treatment is obtained carries out high temperature sintering at last, and temperature is 1800 ℃, and 5 ℃/min of temperature rise rate is incubated 1 hour and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 9
At first adopt bag to mix technology silica flour, ba phenolic resin are mixed with alcohol (mass ratio 1: 1.1: 2), at 80 ℃ of thermal treatment 60min, at 10 ℃ of deepfreeze 60min, injection pressure 1.2MPa, at 90 ℃ of burin-in process 60min,, obtain coat mix powder at 100 ℃ of vacuum-drying 30min; Then with coat mix powder at 100 ℃, 0.2MPa pressure down insulation 30min moulding obtains ceramic green; Then ceramic green (100ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 800 ℃, 0.5 ℃/min of temperature rise rate, insulation 120min; The powder (50ml/min) under argon shield that carbonizing treatment is obtained carries out high temperature sintering at last, and temperature is 1300 ℃, and 1 ℃/min of temperature rise rate is incubated 8 hours and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 10
At first adopt bag to mix technology silica flour, ammonia resol are mixed with alcohol (mass ratio 1: 0.8: 2), at 45 ℃ of thermal treatment 90min, at 5 ℃ of deepfreeze 30min, injection pressure 0.6MPa, at 60 ℃ of burin-in process 90min,, obtain coat mix powder at 60 ℃ of vacuum-drying 90min; Then with coat mix powder at 80 ℃, 0.1MPa pressure down insulation 60min moulding obtains ceramic green; Then ceramic green (100ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 800 ℃, 0.5 ℃/min of temperature rise rate, insulation 120min; At last the powder (50ml/min) under argon shield that obtains after the carbonizing treatment is carried out high temperature sintering, temperature is 1300 ℃, and 1 ℃/min of temperature rise rate is incubated 8 hours and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 11
At first adopt bag to mix technology silica flour, 407 resol are mixed with alcohol (mass ratio 1: 0.5: 2), at 45 ℃ of thermal treatment 90min, at 5 ℃ of deepfreeze 30min, injection pressure 0.6MPa, at 60 ℃ of burin-in process 90min,, obtain coat mix powder at 60 ℃ of vacuum-drying 90min; Then with coat mix powder at 80 ℃, 0.1MPa pressure down insulation 60min moulding obtains ceramic green; Then ceramic green (100ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 600 ℃, 0.5 ℃/min of temperature rise rate, insulation 120min; The powder (50ml/min) under argon shield that carbonizing treatment is obtained carries out high temperature sintering at last, and temperature is 1300 ℃, and 1 ℃/min of temperature rise rate is incubated 8 hours and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 12
At first adopt bag to mix technology silica flour, 401 resol are mixed with alcohol (mass ratio 1: 0.5: 2), at 45 ℃ of thermal treatment 90min, at 5 ℃ of deepfreeze 30min, injection pressure 0.6MPa, at 60 ℃ of burin-in process 90min,, obtain coat mix powder at 60 ℃ of vacuum-drying 90min; Then with coat mix powder at 80 ℃, 0.05MPa pressure down insulation 120min moulding obtains ceramic green; Then ceramic green (50ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 800 ℃, 0.5 ℃/min of temperature rise rate, insulation 120min; The powder (100ml/min) under argon shield that carbonizing treatment is obtained carries out high temperature sintering at last, and temperature is 1600 ℃, and 5 ℃/min of temperature rise rate is incubated 4 hours and forms the porous silicon carbide ceramic with high porosity material.
Embodiment 13
At first adopt bag to mix technology silica flour, ammonia resol are mixed with alcohol (mass ratio 1: 0.5: 2), at 45 ℃ of thermal treatment 90min, at 5 ℃ of deepfreeze 30min, injection pressure 0.6MPa, at 60 ℃ of burin-in process 90min,, obtain coat mix powder at 60 ℃ of vacuum-drying 90min; Then with coat mix powder at 80 ℃, 0.05MPa pressure down insulation 120min moulding obtains ceramic green; Then ceramic green (50ml/min) in argon gas is carried out high temperature cabonization and handle, temperature is 800 ℃, 0.5 ℃/min of temperature rise rate, insulation 120min; The powder that carbonizing treatment is obtained carries out high temperature sintering in a vacuum at last, and temperature is 1600 ℃, and 5 ℃/min of temperature rise rate is incubated 4 hours and forms the porous silicon carbide ceramic with high porosity material.
Claims (2)
1. the preparation method of a porous silicon carbide ceramic with high porosity, described method is a raw material with silica flour, resol and alcohol, after the mixed technology of bag, low-temp low-pressure moulding, high temperature cabonization processing and four step process of high temperature sintering, obtain the porous silicon carbide ceramic with high porosity material, it is characterized in that: concrete processing step is:
1) by the mass ratio 1 of silica flour, resol and alcohol: (0.25~1.1): 2 are mixed into slurry;
2) preparation coat mix powder: mixed slurry is heat-treated at 30~80 ℃, and stir 30~120min; Be cooled to then below 10 ℃, 10~60min is stirred in deepfreeze in 0~10 ℃ of scope simultaneously again; Mixed slurry is injected in the entry injection pressure 0.2~1.2MPa; And carry out burin-in process, churning time 30~120min at 30~90 ℃; The vacuum-drying temperature is 40~100 ℃, and be 30~120min time of drying, obtains the powder that the resol bag mixes silica flour;
3) powder that the resol bag is mixed silica flour is at the low-temp low-pressure molding ceramic green: 60~100 ℃ of mold temperatures; Forming pressure 0.05~0.2MPa; Soaking time 30~120min obtains ceramic green;
4) carbonizing treatment of ceramic green: 600~1000 ℃ of carbonization temperatures; 0.3~1 ℃/min of temperature rise rate; Argon flow amount 50~200ml/min carries out carbonization to ceramic green under soaking time 1~4h;
5) high temperature sintering is handled: with the ceramic green of carbonizing treatment 1300~1800 ℃ of sintering temperatures; Temperature rise rate 1-5 ℃/min; At flow is the argon shield of 50~200ml/min or under vacuum condition; Soaking time 1~8 hour finally obtains the porous silicon carbide ceramic with high porosity material.
2. the preparation method of a kind of porous silicon carbide ceramic with high porosity according to claim 1, it is characterized in that 2124 resol of 2120 resol that described resol as binding agent is Xinhua Resin Factory, Shanghai, 214 resol, Changchun chemical industry two factories, 401 resol and 407 resol of Tianjin resin processing plant, Suzhou resin processing plant and the ammonia resol of Beijing 251 factories and in the ba phenolic resin any one.
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