WO2007056895A1 - Thyrite expansee compacte haute intensite et procede de preparation correspondant - Google Patents

Thyrite expansee compacte haute intensite et procede de preparation correspondant Download PDF

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WO2007056895A1
WO2007056895A1 PCT/CN2005/001962 CN2005001962W WO2007056895A1 WO 2007056895 A1 WO2007056895 A1 WO 2007056895A1 CN 2005001962 W CN2005001962 W CN 2005001962W WO 2007056895 A1 WO2007056895 A1 WO 2007056895A1
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Prior art keywords
silicon carbide
foam
slurry
dense
temperature
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PCT/CN2005/001962
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English (en)
Chinese (zh)
Inventor
Jinsong Zhang
Xiaoming Cao
Chong Tian
Zhenming Yang
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Institute Of Metal Research Chinese Academy Of Sciences
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Priority to PCT/CN2005/001962 priority Critical patent/WO2007056895A1/fr
Publication of WO2007056895A1 publication Critical patent/WO2007056895A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3826—Silicon carbides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance

Definitions

  • the present invention relates to a foamed silicon carbide ceramic material, and more particularly to a high strength dense foamed silicon carbide ceramic material and a method of preparing the same.
  • Foam ceramic is a special porous ceramic.
  • the geometrical feature is a three-dimensional connected network formed by connecting the basic closed loops and the basic units. Due to its excellent high temperature resistance, oxidation resistance, acid and alkali corrosion resistance, thermal shock resistance and semiconductor properties, the production and application of foamed silicon carbide ceramics have received extensive attention.
  • the current foamed silicon carbide ceramics are prepared by the following four methods: powder sintering, solid phase reaction sintering, silicone-containing pyrolysis, and vapor deposition.
  • the powder sintering process is further divided into two different processes.
  • One is to adjust the silicon carbide powder containing a certain amount of sintering aid and the connecting agent (such as ethyl silicate hydrolyzate, silica sol, etc.) into a slurry of suitable concentration, and then immersed in the polyurethane foam, and solidified and dried.
  • the linker and the polyurethane foam are removed in the range of 200 to 600 °C.
  • the temperature is raised to between 1500 and 2200 ° C for sintering to obtain a foamed silicon carbide ceramic;
  • the other method is to uniformly mix the silicon carbide powder containing the sintering aid with the zeolite foaming agent, and then use Molding or casting method.
  • the blowing agent is removed by melting or gasification, and then sintered at a high temperature to obtain a foamed silicon carbide ceramic.
  • a plant-like foaming agent is uniformly mixed with silicon powder and carbon powder.
  • the foaming agent is obtained by melting or gasifying, and after sintering at a high temperature, a foamed silicon carbide ceramic is obtained.
  • the silicon-containing resin pyrolysis method is to form a silicone gel precursor into a polymer gel, and to remove the organic solvent in the gel to obtain a foam-like silicon-containing resin, which is fully pre-oxidized and then pyrolyzed to obtain a foamed silicon carbide ceramic.
  • the vapor deposition method is a method of depositing silicon carbide onto a reticulated carbon fiber braid by chemical vapor deposition to obtain a foamed silicon carbide ceramic.
  • a high intensity proposed by the applicant of the present invention in the Chinese invention patent application (application number 00110479.9)
  • the silicon carbide foam ceramic and the preparation method thereof make the relative enthalpy of the ceramic ribs reach 90% or more, thereby greatly improving the strength of the foamed silicon carbide ceramic.
  • the residual silicon content in ceramic ribs is too high (generally over 20%), and the uneven distribution limits the improvement of the strength of foamed silicon carbide ceramics, which needs to be further solved.
  • the object of the present invention is to provide a high-strength dense foamed silicon carbide ceramic material and a preparation method thereof.
  • the ceramic ribs prepared by the method have high density (more than 99%) and low residual silicon content (less than 10). %), the structure is uniform, and the strength of the foamed silicon carbide ceramic is significantly improved.
  • the technical solution of the present invention is a high-strength dense foamed silicon carbide foam ceramic material characterized by: 90% to 98% silicon carbide and 10% to 2% silicon by weight fraction.
  • the silicon carbide foam ceramic has a polygonal closed ring as a basic unit, and the basic units are connected to each other to form a three-dimensional connected network; the relative density of the ceramic ribs constituting the polygonal closed ring unit is ⁇ 99%, and the average grain size is 50 ⁇ 10 ⁇ .
  • the preparation method of the dense silicon carbide foam ceramic is characterized in that: the silicon carbide powder, the high-yield carbon resin is used as a basic raw material, and the foam plastic is used as a template, and the preparation process is as follows:
  • the silicon carbide powder, the high-yield carbon resin, the curing agent and the ethanol are mixed in proportion, and the weight percentage between the silicon carbide powder, the high-yield carbon resin and the curing agent is 80 wt% to 30 wt%: 19 wt% to 50 wt%: lwt% ⁇ 20wt%, after mechanical agitation, ball milling time is 0.5 ⁇ 2 hours, filtered through 35 ⁇ 140 mesh screen to obtain slurry, solid matter in the slurry (ie solute, including: silicon carbide powder, high yield carbon rate resin and curing
  • the weight of the agent is 30 ⁇ 80% of the total amount of the paddle ;
  • the silicon carbide foam ceramic precursor into a high-pressure container, 'fill with nitrogen or inert gas for high temperature and high pressure curing, the pressure is l ⁇ 35MPa, the temperature is 50 ⁇ 300°C, the heating rate is 1 ⁇ 5°C, the heat preservation is 5 Minutes to 3 hours, obtaining a dense foamed silicon carbide foam ceramic precursor;
  • the dense silicon carbide foam ceramic precursor is pyrolyzed under the protection of nitrogen or an inert atmosphere, the heating rate is 1 ⁇ 5 ° C per minute, the temperature is raised to 600 ⁇ 1300 ° C, and the temperature is kept for 0.5 ⁇ 2 hours to obtain a foam ceramic carbon skeleton; -
  • the foam Since the foam is burned off after pyrolysis, a central hole is left in the foamed ceramic carbon skeleton rib, so it is necessary to fill the carbon skeleton center hole to achieve densification.
  • the filling slurry After the center hole of the surface of the carbon skeleton is ground, the filling slurry is pressed into the center hole by a high pressure injection method, and the pressure is 1 to 35 MPa, and the pressure is maintained for 10 minutes to 2 hours, and the dense foamed silicon carbide is obtained by pyrolysis.
  • Carbon skeleton, pyrolysis is carried out under nitrogen or an inert atmosphere or under vacuum, the heating rate is 10 ° C per minute, the temperature is 600 ⁇ 1300 ° C, and the temperature is maintained for 0.5 to 2 hours;
  • the pyrolyzed dense silicon carbide foam carbon skeleton is reacted and sintered into silicon, and the silicon infiltration is carried out under nitrogen or an inert atmosphere or under vacuum, and the heating rate is 5 to 15 ° C per minute, and the temperature is 1400 to 2000 ° C. Insulation for 0.5 to 4 hours gives high strength dense foamed silicon carbide ceramic material.
  • the high-yield carbon-rate resin is selected from one or more of an epoxy resin, a phenol resin, a furfural resin, and a phenolphthalal resin.
  • the ethanol concentration was 95%. ⁇
  • the silicon carbide powder is a silicon carbide powder having an average particle size of 10 ⁇ to 15 ⁇ .
  • the silicon carbide powder has a weight purity of 95% or more.
  • the curing agent is one of p-toluenesulfonic acid, penolol, oxalic acid or citric acid.
  • the foam is a polyurethane foam or a polyether foam, and has a pore diameter of l to 3 mm.
  • the invention combines a silicon carbide powder with a high-yield carbon-rate resin to prepare a slurry; select a foam of a suitable pore size, and cut it into a desired shape and size, and then immerse it in the slurry, take it out, and use the extrusion, Wind blowing, centrifugation, etc.
  • the ceramic ribs have high density, uniform microstructure and less residual silicon.
  • the method of using the hot-pressed foam ceramic skeleton precursor of the invention not only significantly improves the foam ceramic precursor
  • the initial density of the body ribs also eliminates the problem of microstructure non-uniformity caused by the delamination formed by multiple immersion; and the injection of silicon carbide slurry into the central hole of the foam ceramic carbon skeleton by the injection method, and through the silicon infiltration
  • the reaction is such that the center hole is 3 ⁇ 4 full of silicon carbide.
  • the use of these two measures keeps the density of ceramic ribs above 99%, the residual silicon content below 10% (generally below 5%), and the microstructure is very uniform, see Figures 1, 2, and 3. This is a remarkable feature not found in other foamed silicon carbide ceramic preparation methods.
  • the compressive strength reaches 500 MPa, cm 3 1 , which is more than 2 times higher than the compressive strength of the foamed silicon carbide ceramic prepared by the method of the present invention (Application No. 00110479.9), which is prepared by other methods.
  • the foamed silicon carbide ceramic 3 ⁇ 4 has a 5 to 10 times higher compressive strength.
  • Figure 1 shows the macroscopic morphology of the foamed silicon carbide ceramic (scale is lmm).
  • Figure 2 shows the fracture morphology of the foamed silicon carbide ceramic rib (200 ⁇ scale).
  • Figure 3 shows the microstructure inside the foamed silicon carbide ceramic rib (scale 50 ⁇ m).
  • the weight ratio is 60%: 35%: 5% of the average particle size 2 ⁇ silicon carbide powder, ammonia phenolic resin, p-toluenesulfonic acid co-dissolved in absolute ethanol, so that the solids in the slurry: silicon carbide powder, high carbon production
  • the weight of the resin and the curing agent is 40% of the total amount of the slurry, and the ball milling time is 0.5 hour after mechanical stirring, and filtered through a 35 mesh screen to prepare a slurry, and the polyurethane foam having a pore diameter of 1 mm is cut into a required size.
  • the precursor was pyrolyzed under argon gas to form a carbon skeleton; wherein the heating rate was 2 ° C per minute, the temperature was raised to 800 Torr, and the temperature was maintained for 0.5 hours.
  • the center hole of the surface of the carbon skeleton is ground, and a slurry having a viscosity of 150 mPa-s is pressed into the center hole in a high-pressure vessel at a pressure of 5 MPa. After holding for 20 minutes, it is pyrolyzed under argon gas to heat up. The rate is 2 ⁇ per minute, the temperature is 800°C, and the temperature is kept for 0.5 hours.
  • a high-strength dense silicon carbide foam ceramic material having a rib density of 99%, a residual silicon content of 5%, a silicon carbide average grain size of 1.8 ⁇ , and a foamed silicon carbide ceramic specific compressive strength of 460 ⁇ 3 ⁇ 3 ⁇ , The composition is silicon carbide: 98%, silicon: 2%.
  • Embodiment 1 The difference from Embodiment 1 is:
  • the weight ratio is 45%: 50%: 5% of the average particle size of 2 ⁇ silicon carbide powder, epoxy resin (brand number EP0141 - 310), p-toluenesulfonic acid co-dissolved in anhydrous ethanol, so that the solids in the slurry :
  • the weight of silicon carbide powder, high-yield carbon resin and curing agent is 60% of the total amount of slurry.
  • the ball milling time is 1 hour, filtered through a 55 mesh screen to prepare a slurry, and a polyamine with a pore diameter of 2 mm.
  • the fat foam After the fat foam is cut into the required size, it is evenly immersed in the slurry, soaked for 1 minute, taken out and squeezed out the excess slurry, air-dried, and semi-cured at 50 ° C for 10 minutes. The above process is repeated several times until it reaches The required weight of 20% of the predetermined volume fraction (volume fraction of the silicon carbide ceramic in the finished product). Then, it was placed in a high-pressure vessel, filled with nitrogen gas to a pressure of 10 MPa, and the temperature was raised to 200 ° C, and the temperature was raised to 3 Torr per minute, and the temperature was maintained for 1 hour.
  • the solution is pyrolyzed under argon gas protection at a heating rate of 3 ° C per minute, temperature 900 ° C, holding for 1 hour; after pyrolysis, vacuum siliconizing, reaction temperature 1600 ° C, heating rate of 10 ⁇ / min, holding for 1 hour, to obtain high strength dense silicon carbide foam ceramic material , the rib density is 99 ° /.
  • the average grain size of silicon carbide is 1.7 ⁇ , and its composition is silicon carbide: 95%, silicon: 5%.
  • Embodiment 1 The difference from Embodiment 1 is:
  • the polyurethane foam with a pore size of 2 mm was cut into the required size and uniformly immersed in the slurry. After taking out, the excess slurry was squeezed out, soaked for 1 minute, and air-dried and semi-cured at 60 ° C for 50 minutes. The above process was repeated several times. , until the desired weight fraction of 40% of the predetermined volume fraction (the volume fraction of the silicon carbide ceramic in the finished product) is reached. It was placed in a high-pressure vessel, filled with nitrogen gas to a pressure of ll MPa, and heated to 230 ° C. The heating rate was 4 ° C per minute and the temperature was maintained for 15 minutes.
  • the silicon carbide foam ceramic material has a rib density of 99%, and the silicon carbide has an average grain size of 4.2 ⁇ m, and its composition is silicon carbide: 92%, silicon: 8%.
  • the difference from the first embodiment is that - the weight ratio of 60%: 35%: 5% of the average particle size of 1.5 ⁇ m silicon carbide powder, boron phenolic resin, and pentazol are co-dissolved in absolute ethanol to make the slurry
  • Medium solids The weight of silicon carbide powder, high-yield carbon resin and curing agent is 80% of the total volume of the paddle. After mechanical agitation, the ball milling time is 0.5 hours. After filtering through a 95 mesh screen, the slurry is made into a slurry with a pore size of 2 mm.
  • the polyurethane foam is cut into the required size and uniformly immersed in the slurry, soaked for 1 minute, taken out and squeezed out the excess slurry, and the air is semi-cured at 80 ° C for 20 minutes, and the above process is repeated several times until The weight required to reach 50% of the predetermined volume fraction (volume fraction of silicon carbide ceramics in the finished product). It was placed in a high-pressure vessel, filled with argon gas to a pressure of 18 MPa, raised to 260 ° C, and heated at a rate of 5 ° C per minute for 2 hours.
  • the dense dense silicon carbide foam ceramic material has a rib density of 100%, and the average grain size of the silicon carbide is ⁇ . ⁇ , and its composition is silicon carbide: 90%, silicon: 10%.
  • Embodiment 1 The difference from Embodiment 1 is:
  • Silicon carbide powder resin (60% of thermosetting phenolic resin, 40% of bismuth resin) and penolsine weight ratio of 50wt%: 30wt%: 20wt%, co-solvent of thermosetting phenolic resin and furfural resin with penolidine
  • resin 60% of thermosetting phenolic resin, 40% of bismuth resin
  • penolsine weight ratio 50wt%: 30wt%: 20wt%
  • the solid content of the slurry the weight of the silicon carbide powder, the high-yield carbon resin and the curing agent are 30% of the total amount of pulp
  • the ball milling time is 1 hour, filtered through a 120 mesh screen to form a slurry, and the polyurethane foam having a pore diameter of 2 mm is cut into a desired size and uniformly immersed in the slurry.
  • Soak for 1 minute take out the excess slurry, and dry it at 50 °C for 30 minutes. The above process is repeated several times until it reaches 60% of the predetermined volume fraction (SiC silicon carbide in the finished product).
  • the volume fraction of porcelain is the required weight.
  • Put it into a high-pressure container fill it with nitrogen gas to bring the pressure to 25 MPa, raise the temperature to 240, and raise the temperature by 2 ⁇ per minute, and heat it for 1 hour. Pyrolysis under argon gas to form a carbon skeleton; wherein the heating rate is 4 ° C per hour, the temperature is raised to 1000 ° C, and the temperature is maintained for 0.5 hours.
  • the center hole of the carbon bone surface is ground.
  • the slurry with a viscosity of 180 mPa's is pressed into the center hole at a pressure of 20 MPa.
  • the solution is pyrolyzed under argon gas protection at a heating rate of 6 ° C per minute, temperature 600 ° C, holding for 2 hours; after pyrolysis, vacuum siliconizing, reaction temperature 550 ° C, heating rate of 15 ° C / min, holding for 1 hour, high strength dense silicon carbide
  • the foamed ceramic material has a rib density of 99%, and the average grain size of the silicon carbide is 3.8 ⁇ m, and its composition is silicon carbide: 96%, silicon: 4%.
  • Embodiment 1 The difference from Embodiment 1 is:
  • Silicon carbide powder resin (thermosetting phenolic resin 50%, furfural resin 50%) and citric acid weight ratio 40wt%: 40wt%: 20wt%, cosolving thermosetting phenolic resin and furfural resin with citric acid in absolute ethanol,
  • the slurry solution is prepared, and the silicon carbide powder having an average particle size of ⁇ is uniformly added to the above solution to make the solid content in the slurry: the weight of the silicon carbide powder, the high-yield carbon resin and the curing agent is 80% of the total amount of the slurry.
  • the ball milling time is 2 hours, filtered through a 140 mesh screen to prepare a slurry.
  • the polyurethane foam having a pore size of 3 mm is cut into the required size and uniformly immersed in the slurry, soaked for 1 minute, and taken out. After the excess paddle is squeezed out and air-dried for 10 minutes at 50 ° C, the above process is repeated several times until the desired weight of 10% of the predetermined volume fraction (the volume fraction of the silicon carbide ceramic in the finished product) is reached. It is placed in a high-pressure vessel, filled with nitrogen gas to a pressure of 20 MPa, and heated to 280 ° C. The heating rate is 5 ° C per minute and the temperature is maintained for 1 hour.
  • the slurry is pyrolyzed under argon gas protection at a heating rate of 5 ° C per minute, temperature 800 ° C, heat preservation for 2 hours; after pyrolysis, vacuum silicon infiltration, reaction temperature 1650 ° C, heating rate of 15 ° C / min, heat preservation for 1 hour, to obtain high strength dense silicon carbide foam
  • the ceramic material has a rib density of 100%, and the silicon carbide has an average grain size of 7.2 ⁇ m, and its composition is silicon carbide: 94%, silicon: 6%.

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
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  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
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Abstract

Cette invention concerne un matériau céramique à base de carbure de silicium expansé compact présentant une grande résistance, ainsi qu'un procédé permettant de produire un tel matériau. Le matériau susmentionné est composé de 90 à 98% en poids de carbure de silicium et de 10 à 20% en poids de silicium. Selon le mode de réalisation décrit dans cette invention, la poudre de carbure de silicium et la résine présentant un taux de production de carbone élevé sont mélangés de manière à former une boue; du plastique alvéolaire est découpé puis trempé dans la boue, puis retiré de la boue afin d'éliminer l'excédent de bout; ensuite, le plastique alvéolaire est traité par semi-solidification, puis par solidification à haute température et haute pression, le corps alvéolaire solidifié est pyrolysé de manière à obtenir un cadre en carbone alvéolaire présentant la même forme que la forme alvéolaire d'origine, lequel corps est constitué de carbure de silicium et de carbone pyrolysé. Le procédé consiste ensuite à ouvrir un orifice central sur le cadre en carbone par dépolissage. La boue à base de carbure de silicium est injectée dans l'orifice central jusqu'à remplissage complet par injection par pression, puis elle est pyrolysée; le carbone contenu dans le cadre de carbone réagit avec le silicium dans une phase gazeuse ou liquide grâce à un processus d'infiltration de manière à produire du carbure de silicium qui est ensuite combiné avec des particules de carbure de silicium d'origine dans le matériau céramique contenant le cadre de carbure de silicium compact avec une résistance importante. Le réseau céramique ainsi obtenu présente une microstructure homogène haute densité et une plus petite quantité de résidus de silicium.
PCT/CN2005/001962 2005-11-18 2005-11-18 Thyrite expansee compacte haute intensite et procede de preparation correspondant WO2007056895A1 (fr)

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CN104418593A (zh) * 2013-08-20 2015-03-18 沈阳铝镁科技有限公司 一种耐高温、耐冲刷材料及其制备方法
CN104924412A (zh) * 2015-05-26 2015-09-23 中国科学院长春光学精密机械与物理研究所 反应烧结碳化硅陶瓷素坯的连接方法
CN110790579A (zh) * 2019-12-04 2020-02-14 冷水江市鑫达耐火材料制造有限公司 一种无铬耐火砖及其制备方法
CN113698215A (zh) * 2020-05-20 2021-11-26 中国科学院金属研究所 一种致密的层状碳化硅陶瓷及其制备方法
US20220173372A1 (en) * 2010-12-22 2022-06-02 Enevate Corporation Electrodes, electrochemical cells, and methods of forming electrodes and electrochemical cells
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US20220173372A1 (en) * 2010-12-22 2022-06-02 Enevate Corporation Electrodes, electrochemical cells, and methods of forming electrodes and electrochemical cells
US11710814B2 (en) * 2010-12-22 2023-07-25 Enevate Corporation Electrodes, electrochemical cells, and methods of forming electrodes and electrochemical cells
CN102537510A (zh) * 2010-12-31 2012-07-04 张光荣 无压烧结碳化硅陶瓷阀芯及其制备工艺
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CN104418593B (zh) * 2013-08-20 2016-09-07 沈阳铝镁科技有限公司 一种耐高温、耐冲刷材料及其制备方法
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CN110790579A (zh) * 2019-12-04 2020-02-14 冷水江市鑫达耐火材料制造有限公司 一种无铬耐火砖及其制备方法
CN113698215A (zh) * 2020-05-20 2021-11-26 中国科学院金属研究所 一种致密的层状碳化硅陶瓷及其制备方法
CN113698215B (zh) * 2020-05-20 2022-10-11 中国科学院金属研究所 一种致密的层状碳化硅陶瓷及其制备方法
CN115141028A (zh) * 2022-05-29 2022-10-04 西北工业大学 基于凝胶注模预强化制备碳化硅基复合材料整体涡轮盘的方法
CN115141028B (zh) * 2022-05-29 2023-08-29 西北工业大学 基于凝胶注模预强化制备碳化硅基复合材料整体涡轮盘的方法

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