CN110451976A - A kind of composite material of silicon carbide and preparation method thereof - Google Patents

A kind of composite material of silicon carbide and preparation method thereof Download PDF

Info

Publication number
CN110451976A
CN110451976A CN201910425891.8A CN201910425891A CN110451976A CN 110451976 A CN110451976 A CN 110451976A CN 201910425891 A CN201910425891 A CN 201910425891A CN 110451976 A CN110451976 A CN 110451976A
Authority
CN
China
Prior art keywords
silicon carbide
composite material
temperature
crosslinking
carbide according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201910425891.8A
Other languages
Chinese (zh)
Inventor
刘骏
刘振华
张海
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hunan Prince New Mstar Technology Ltd
Original Assignee
Hunan Prince New Mstar Technology Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hunan Prince New Mstar Technology Ltd filed Critical Hunan Prince New Mstar Technology Ltd
Priority to CN201910425891.8A priority Critical patent/CN110451976A/en
Publication of CN110451976A publication Critical patent/CN110451976A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • C04B35/571—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 obtained from Si-containing polymer precursors or organosilicon monomers
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
    • 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
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
    • 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
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
    • C04B2235/9692—Acid, alkali or halogen resistance

Abstract

The invention discloses a kind of composite material of silicon carbide, as mass fraction, including following components: silicon carbide powder 60~80%, organic metal salt 10~30%, binder 1~15%.The invention also discloses a kind of preparation methods of composite material of silicon carbide, comprising: is ultrasonically treated silicon carbide powder, organic metal salt and binder；Uniformly mixed raw material is put into crosslinking pyrolysis furnace, under the protection of argon gas, the temperature of the crosslinking pyrolysis furnace is warming up to 1000 DEG C from 200 DEG C with the heating rate of 1~2 DEG C/min, and keep the temperature 2~3h at 1000 DEG C；The solid matter that crosslinking cracking obtains is subjected to ball milling；Under protection of argon gas, solid matter ball milling obtained, which is put into high temperature heat treatment furnace, to be heat-treated, and composite material of silicon carbide is obtained.Composite material of silicon carbide prepared by the present invention has the advantages that excellent antiseptic property, heat transfer efficiency, oxidation resistance, and effectively reduces cost.

Description

A kind of composite material of silicon carbide and preparation method thereof
Technical field
The present invention relates to carbofrax material technical fields, it is more particularly related to a kind of composite material of silicon carbide And preparation method thereof.
Background technique
Silicon carbide (SiC) ceramics have thermal expansion coefficient is small, decomposition temperature is high, density low and high temperature intensity is high, it is corrosion-resistant, The excellent properties such as wear-resistant, resistance to ablation are used extensively in 1300 DEG C of one of most promising high-temperature structural materials used above In heat-resisting, wear-resisting and harsh use environment occasion.
There are oxidative phenomena when SiC ceramic applied at elevated temperature, oxidation mechanism is divided into actively oxidation and passive oxidation.High temperature is low Occur actively to aoxidize when partial pressure of oxygen, SiC material oxidation generates the SiO of volatilization, causes quality of materials to reduce, then material failure. Passive oxidation occurs when medium temperature high keto sectional pressure, SiC material aoxidizes to form SiO2Thinfilm protective coating prevents oxygen from internally spreading, material Expect that quality increases.The SiO that SiC material is formed in passive oxidation mechanism lower surface2Film oxygen resistance is good, and oxygen diffusion rate is much low In other high-temperature oxides, thus the use of effective protection SiC at high temperature.Under certain partial pressure of oxygen environment, two kinds of oxidations There are temperature transition points for mechanism, and oxidation mechanism is become actively aoxidizing from passive oxidation when material surface temperature is higher than inversion temperature, The use temperature of the inversion temperature control silicon carbide of main passive oxidation.
For SiC material as structure member, such as space flight aircraft, working environment is high-temperature low-oxygen partial pressure, Yi Fasheng It actively aoxidizes, material failure, it is therefore desirable to which carbofrax material uses temperature with higher.Due to SiO2It is divided in high-temperature low-oxygen When actively volatilize, so, at present majority silicon carbide use temperature be about 1700 DEG C, limit its use scope, it is necessary to open New method is sent out to prepare silicon carbide, improves the inversion temperature of its main passive oxidation, to improve silicon carbide using temperature, is obtained resistance to High temperature, anti-oxidant, inexpensive carbofrax material.
Summary of the invention
It is an object of the invention to solve at least the above problems, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide one kind can be further improved antiseptic property, improves heat transfer efficiency, enhancing The high-temperature stability of silicon, the composite material of silicon carbide for reducing oxidation efficiency and reducing cost and preparation method thereof.
To achieve the goals above, the invention discloses a kind of composite material of silicon carbide, as mass fraction, including it is following Component:
Silicon carbide powder 60~80%, organic metal salt 10~30%, binder 1~15%.
Preferably, in the present invention, the organic metal salt is acetylacetone,2,4-pentanedione potassium or potassium isopropoxide.
Preferably, in the present invention, the binder is waterborne organic silicon resin or oligomeric silane.
Preferably, in the present invention, the waterborne organic silicon resin is poly- methyl silicon resin or poly- ethyl silicone resin.
Preferably, the present invention in, the oligomeric silane be 3- methacryloxypropyl three (trimethylsiloxy group) silane, Any one in phenyl three (dimethylsilyl bis) silane, 1,3- diphenyl four (dimethylsilyl bis) disiloxane.
Preferably, in the present invention, the partial size of the silicon carbide powder is 0.1~100 μm.
The invention also discloses a kind of preparation methods of composite material of silicon carbide, comprising the following steps:
Step 1: as mass fraction, by 60~80% silicon carbide powder, 10~30% organic metal salt and 1~ 15% binder is ultrasonically treated；
Step 2: uniformly mixed raw material is put into crosslinking pyrolysis furnace, under the protection of argon gas, with 1~2 DEG C/min's The temperature of the crosslinking pyrolysis furnace is warming up to 1000 DEG C from 200 DEG C by heating rate, and 2~3h is kept the temperature at 1000 DEG C；
Step 3: the solid matter that crosslinking cracking obtains is carried out ball milling；
Step 4: under protection of argon gas, the solid matter that ball milling is obtained, which is put into high temperature heat treatment furnace, carries out hot place Reason, heat treatment temperature are 1800~1900 DEG C, and the processing time is 1~2h, obtains composite material of silicon carbide.
Preferably, in the present invention, the frequency of the ultrasonic treatment is 100KHz, ultrasonic time 1h.
Preferably, in the present invention, in the step 3, Ball-milling Time is 1~3h, rotational speed of ball-mill 1000r/min.
The present invention, by introducing micro metal elemental lithium in silicon carbide, passes through high temperature using silicon carbide powder as raw material Heat treatment process realizes being sufficiently mixed and reacting completely for metallic potassium and silicon carbide.After curing reaction, it is capable of forming jail Solid chemical bond, during passive oxidation, formed metal silicon/silicon dioxide solid solution, reduce the activity of silica, hence it is evident that mention The high inversion temperature of main passive oxidation, to form composite material of silicon carbide resistant to high temperature, and effectively reduces material cost.
The present invention, as binder, is capable of providing carbon source and silicon source using waterborne organic silicon resin or oligomeric silane, In crosslinking pyrolysis furnace, waterborne organic silicon resin or oligomeric silane occur to crack and form silicon carbide, and through pervaporation and cohesion Effect deposits on silicon carbide powder, forms compacted zone, to ensure that the density of silicon carbide, and reduces oxidation probability.
The present invention is include at least the following beneficial effects:
1, composite material of silicon carbide provided by the invention effectively increases resistance to height by introducing lithium metal in silicon carbide Temperature, Corrosion Protection, enhance the high-temperature stability of silicon, and reduce oxidation probability, significantly reduce cost.
2, composite material of silicon carbide provided by the invention has homogeneity, and the doping of metallic potassium does not change the macro of silicon carbide Structure is seen, the physical property of silicon carbide is had no significant effect.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification Text can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein are not precluded one or more The presence or addition of a other elements or combinations thereof.
Embodiment 1
The invention discloses a kind of composite material of silicon carbide, as mass fraction, comprising: silicon carbide powder 80%, acetyl Acetone potassium 15%, poly- methyl silicon resin 5%.The partial size of silicon carbide powder is 100 μm.
The preparation method of composite material of silicon carbide described above the following steps are included:
Step 1: 80% silicon carbide powder, 15% acetylacetone,2,4-pentanedione potassium and 5% poly- methyl silicon resin are carried out ultrasound Processing, the frequency of ultrasonic treatment are 100KHz, ultrasonic time 1h；
Step 2: uniformly mixed raw material is put into crosslinking pyrolysis furnace, under the protection of argon gas, with the liter of 1 DEG C/min The temperature of the crosslinking pyrolysis furnace is warming up to 1000 DEG C from 200 DEG C by warm rate, and keeps the temperature 2h at 1000 DEG C；
Step 3: the solid matter that crosslinking cracking obtains is carried out ball milling, Ball-milling Time 2h, rotational speed of ball-mill 1000r/ min；
Step 4: under protection of argon gas, the solid matter that ball milling is obtained, which is put into high temperature heat treatment furnace, carries out hot place Reason, heat treatment temperature are 1800 DEG C, and the processing time is 2h, obtains composite material of silicon carbide.
Performance test is carried out to the composite material of silicon carbide of preparation, test result is composite material of silicon carbide at 1900 DEG C Ablating rate is 0.015% under aerobic environment, and in corrosive liquid, corrosivity weightlessness is 0.16mg/cm3, corrosive liquid is by volume basis The HNO that concentration is 10%HF and concentration expressed in percentage by volume is 57%310:1 is formed by volume, density 3.08g/cm3.1950 Still have excellent antioxygenic property and corrosion resistance under DEG C high temperature.
Embodiment 2
The invention discloses a kind of composite material of silicon carbide, as mass fraction, comprising: silicon carbide powder 70%, isopropyl Potassium alcoholate 20%, poly- ethyl silicone resin 10%.The partial size of silicon carbide powder is 50 μm.
The preparation method of above-mentioned composite material of silicon carbide the following steps are included:
Step 1: as mass fraction, by 70% silicon carbide powder, 20% potassium isopropoxide and 10% poly- ethyl silicon Resin is ultrasonically treated, and the frequency of ultrasonic treatment is 100KHz, ultrasonic time 1h；
Step 2: uniformly mixed raw material is put into crosslinking pyrolysis furnace, under the protection of argon gas, with the liter of 2 DEG C/min The temperature of the crosslinking pyrolysis furnace is warming up to 1000 DEG C from 200 DEG C by warm rate, and keeps the temperature 3h at 1000 DEG C；
Step 3: the solid matter that crosslinking cracking obtains is carried out ball milling, Ball-milling Time 3h, rotational speed of ball-mill 1000r/ min；
Step 4: under protection of argon gas, the solid matter that ball milling is obtained, which is put into high temperature heat treatment furnace, carries out hot place Reason, heat treatment temperature are 1900 DEG C, and the processing time is 1h, obtains composite material of silicon carbide.
Performance test is carried out to the composite material of silicon carbide of preparation, test result is composite material of silicon carbide at 1900 DEG C Ablating rate is 0.014% under aerobic environment, and in corrosive liquid, corrosivity weightlessness is 0.14mg/cm3, corrosive liquid is by volume basis The HNO that concentration is 10%HF and concentration expressed in percentage by volume is 57%310:1 is formed by volume, density 3.06g/cm3.1950 Still have excellent antioxygenic property and corrosion resistance under DEG C high temperature.
Embodiment 3
The invention discloses a kind of composite material of silicon carbide, as mass fraction, comprising: silicon carbide powder 60%, acetyl Acetone potassium 30%, 3- methacryloxypropyl three (trimethylsiloxy group) silane 10%.The partial size of silicon carbide powder is 20 μm.
The preparation method of above-mentioned composite material of silicon carbide the following steps are included:
Step 1: by 60% silicon carbide powder, 30% acetylacetone,2,4-pentanedione potassium and 10% 3- methacryloxypropyl Three (trimethylsiloxy group) silane are ultrasonically treated, and the frequency of ultrasonic treatment is 100KHz, ultrasonic time 1h；
Step 2: uniformly mixed raw material is put into crosslinking pyrolysis furnace, under the protection of argon gas, with 1.5 DEG C/min's The temperature of the crosslinking pyrolysis furnace is warming up to 1000 DEG C from 200 DEG C by heating rate, and keeps the temperature 2.5h at 1000 DEG C；
Step 3: the solid matter that crosslinking cracking obtains is carried out ball milling, Ball-milling Time 2h, rotational speed of ball-mill 1000r/ min；
Step 4: under protection of argon gas, the solid matter that ball milling is obtained, which is put into high temperature heat treatment furnace, carries out hot place Reason, heat treatment temperature are 1800 DEG C, and the processing time is 2h, obtains composite material of silicon carbide.
Performance test is carried out to the composite material of silicon carbide of preparation, test result is composite material of silicon carbide at 1900 DEG C Ablating rate is 0.013% under aerobic environment, and in corrosive liquid, corrosivity weightlessness is 0.13mg/cm3, corrosive liquid is by volume basis The HNO that concentration is 10%HF and concentration expressed in percentage by volume is 57%310:1 is formed by volume, density 3.09g/cm3.1950 Still have excellent antioxygenic property and corrosion resistance under DEG C high temperature.
Embodiment 4
The invention discloses a kind of composite material of silicon carbide, as mass fraction, comprising: silicon carbide powder 65%, isopropyl Potassium alcoholate 20%, 3- methacryloxypropyl three (trimethylsiloxy group) silane 15%.The partial size of silicon carbide powder is 0.1 μm.
The preparation method of above-mentioned composite material of silicon carbide the following steps are included:
Step 1: as mass fraction, by 65% silicon carbide powder, 20% potassium isopropoxide and 15% 3- methyl-prop Alkene monomethacryloxypropyl three (trimethylsiloxy group) silane is ultrasonically treated, and the frequency of ultrasonic treatment is 100KHz, and ultrasonic time is 1h；
Step 2: uniformly mixed raw material is put into crosslinking pyrolysis furnace, under the protection of argon gas, with 1~2 DEG C/min's The temperature of the crosslinking pyrolysis furnace is warming up to 1000 DEG C from 200 DEG C by heating rate, and 2~3h is kept the temperature at 1000 DEG C；
Step 3: the solid matter that crosslinking cracking obtains is carried out ball milling, Ball-milling Time 2.5h, rotational speed of ball-mill is 1000r/min；
Step 4: under protection of argon gas, the solid matter that ball milling is obtained, which is put into high temperature heat treatment furnace, carries out hot place Reason, heat treatment temperature are 1800 DEG C, and the processing time is 1.5h, obtains composite material of silicon carbide.
Performance test is carried out to the composite material of silicon carbide of preparation, test result is composite material of silicon carbide at 1900 DEG C Ablating rate is 0.013% under aerobic environment, and in corrosive liquid, corrosivity weightlessness is 0.14mg/cm3, corrosive liquid is by volume basis The HNO that concentration is 10%HF and concentration expressed in percentage by volume is 57%310:1 is formed by volume, density 3.07g/cm3.1950 Still have excellent antioxygenic property and corrosion resistance under DEG C high temperature.
Embodiment 5
The invention discloses a kind of composite material of silicon carbide, as mass fraction, comprising: silicon carbide powder 75%, acetyl Acetone potassium 17%, phenyl three (dimethylsilyl bis) silane 8%.The partial size of silicon carbide powder is 10 μm.
The preparation method of above-mentioned composite material of silicon carbide the following steps are included:
Step 1: as mass fraction, by 75% silicon carbide powder, 17% acetylacetone,2,4-pentanedione potassium and 8% phenyl three (dimethylsilyl bis) silane is ultrasonically treated, and the frequency of ultrasonic treatment is 100KHz, ultrasonic time 1h；
Step 2: uniformly mixed raw material is put into crosslinking pyrolysis furnace, under the protection of argon gas, with the liter of 2 DEG C/min The temperature of the crosslinking pyrolysis furnace is warming up to 1000 DEG C from 200 DEG C by warm rate, and keeps the temperature 2h at 1000 DEG C；
Step 3: the solid matter that crosslinking cracking obtains is carried out ball milling, Ball-milling Time 2.5h, rotational speed of ball-mill is 1000r/min；
Step 4: under protection of argon gas, the solid matter that ball milling is obtained, which is put into high temperature heat treatment furnace, carries out hot place Reason, heat treatment temperature are 1900 DEG C, and the processing time is 1h, obtains composite material of silicon carbide.
Performance test is carried out to the composite material of silicon carbide of preparation, test result is composite material of silicon carbide at 1900 DEG C Ablating rate is 0.014% under aerobic environment, and in corrosive liquid, corrosivity weightlessness is 0.13mg/cm3, corrosive liquid is by volume basis The HNO that concentration is 10%HF and concentration expressed in percentage by volume is 57%310:1 is formed by volume, density 3.09g/cm3.1950 Still have excellent antioxygenic property and corrosion resistance under DEG C high temperature.
Embodiment 6
The invention discloses a kind of composite material of silicon carbide, as mass fraction, comprising: silicon carbide powder 70%, isopropyl Potassium alcoholate 18%, 1,3- diphenyl four (dimethylsilyl bis) disiloxane 12%.The partial size of silicon carbide powder is 80 μm.
The preparation method of above-mentioned composite material of silicon carbide the following steps are included:
Step 1: as mass fraction, by 70% silicon carbide powder, 18% potassium isopropoxide and 12% 1,3- hexichol Base four (dimethylsilyl bis) disiloxane is ultrasonically treated, and the frequency of ultrasonic treatment is 100KHz, ultrasonic time 1h；
Step 2: uniformly mixed raw material is put into crosslinking pyrolysis furnace, under the protection of argon gas, with 1~2 DEG C/min's The temperature of the crosslinking pyrolysis furnace is warming up to 1000 DEG C from 200 DEG C by heating rate, and 2~3h is kept the temperature at 1000 DEG C；
Step 3: the solid matter that crosslinking cracking obtains is carried out ball milling, Ball-milling Time 2h, rotational speed of ball-mill 1000r/ min；
Step 4: under protection of argon gas, the solid matter that ball milling is obtained, which is put into high temperature heat treatment furnace, carries out hot place Reason, heat treatment temperature are 1880 DEG C, and the processing time is 1.5h, obtains composite material of silicon carbide.
Performance test is carried out to the composite material of silicon carbide of preparation, test result is composite material of silicon carbide at 1900 DEG C Ablating rate is 0.013% under aerobic environment, and in corrosive liquid, corrosivity weightlessness is 0.15mg/cm3, corrosive liquid is by volume basis The HNO that concentration is 10%HF and concentration expressed in percentage by volume is 57%310:1 is formed by volume, density 3.08g/cm3.1950 Still have excellent antioxygenic property and corrosion resistance under DEG C high temperature.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details.

Claims (9)

1. a kind of composite material of silicon carbide, which is characterized in that as mass fraction, including following components:
Silicon carbide powder 60~80%, organic metal salt 10~30%, binder 1~15%.
2. composite material of silicon carbide according to claim 1, which is characterized in that the organic metal salt is acetylacetone,2,4-pentanedione potassium Or potassium isopropoxide.
3. composite material of silicon carbide according to claim 1, which is characterized in that the binder is waterborne organic silicon resin Or oligomeric silane.
4. composite material of silicon carbide according to claim 3, which is characterized in that the waterborne organic silicon resin is poly- methyl Silicone resin or poly- ethyl silicone resin.
5. composite material of silicon carbide according to claim 3, which is characterized in that the oligomeric silane is 3- methacryl Oxygen propyl group three (trimethylsiloxy group) silane, phenyl three (dimethylsilyl bis) silane, 1,3- diphenyl, four (dimethyl silica Base) any one in disiloxane.
6. composite material of silicon carbide according to claim 1, which is characterized in that the partial size of the silicon carbide powder is 0.1 ~100 μm.
7. a kind of method for preparing described in any item composite material of silicon carbide according to claim 1~6, which is characterized in that packet Include following steps:
Step 1: as mass fraction, by 60~80% silicon carbide powder, 10~30% organic metal salt and 1~15% Binder be ultrasonically treated；
Step 2: uniformly mixed raw material is put into crosslinking pyrolysis furnace, under the protection of argon gas, with the heating of 1~2 DEG C/min The temperature of the crosslinking pyrolysis furnace is warming up to 1000 DEG C from 200 DEG C by rate, and 2~3h is kept the temperature at 1000 DEG C；
Step 3: the solid matter that crosslinking cracking obtains is carried out ball milling；
Step 4: under protection of argon gas, the solid matter that ball milling is obtained, which is put into high temperature heat treatment furnace, to be heat-treated, heat Treatment temperature is 1800~1900 DEG C, and the processing time is 1~2h, obtains composite material of silicon carbide.
8. a kind of preparation method of composite material of silicon carbide according to claim 7, which is characterized in that the ultrasonic treatment Frequency be 100KHz, ultrasonic time 1h.
9. a kind of preparation method of composite material of silicon carbide according to claim 7, which is characterized in that the step 3 In, Ball-milling Time is 1~3h, rotational speed of ball-mill 1000r/min.
CN201910425891.8A 2019-05-21 2019-05-21 A kind of composite material of silicon carbide and preparation method thereof Withdrawn CN110451976A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910425891.8A CN110451976A (en) 2019-05-21 2019-05-21 A kind of composite material of silicon carbide and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910425891.8A CN110451976A (en) 2019-05-21 2019-05-21 A kind of composite material of silicon carbide and preparation method thereof

Publications (1)

Publication Number Publication Date
CN110451976A true CN110451976A (en) 2019-11-15

Family

ID=68480987

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910425891.8A Withdrawn CN110451976A (en) 2019-05-21 2019-05-21 A kind of composite material of silicon carbide and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110451976A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114195519A (en) * 2020-09-17 2022-03-18 山东硅纳新材料科技有限公司 Precursor converted silicon carbide ceramic and preparation method thereof
CN114248342A (en) * 2022-02-07 2022-03-29 东莞市志橙半导体材料有限公司 Preparation method of special-shaped semiconductor tube core non-conductive protection tube

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114195519A (en) * 2020-09-17 2022-03-18 山东硅纳新材料科技有限公司 Precursor converted silicon carbide ceramic and preparation method thereof
CN114248342A (en) * 2022-02-07 2022-03-29 东莞市志橙半导体材料有限公司 Preparation method of special-shaped semiconductor tube core non-conductive protection tube

Similar Documents

Publication Publication Date Title
CN103469207B (en) High-temperature oxidation resistant and corrosion resistant glass ceramic composite coating and preparation technology thereof
CN102277560B (en) Method for improving oxidation resistance of graphite electrode by obtaining SiC/C gradient surface coating through chemical vapor deposition
CN100577892C (en) Water heat electrophoresis deposition method of gradient iridium silicate coating layer
Bezzi et al. SiC/MoSi2 based coatings for Cf/C composites by two step pack cementation
CN106977223A (en) C/C composites ceramic modified and with ceramic coating and preparation method thereof
CN110451976A (en) A kind of composite material of silicon carbide and preparation method thereof
US9259760B2 (en) Method for coating oxidation protective layer for carbon/carbon composite, carbon heater, and cooker
CN103265331B (en) C/SiC/Na2SiO3 antioxidative compound coating suitable for graphite material and preparation method thereof
CN106587629B (en) Boride modified glass ceramic base combined high temperature antioxidant coating and preparation method thereof
CN103774435A (en) Preparation and application methods of carbon fiber mat surface antioxidation coating
CN106221559A (en) A kind of ordinary steel high-temp. resistant antioxidation coating and using method thereof
CN102249235B (en) Method for preparing high-temperature resistant silicon carbide
CN100546940C (en) A kind of method for preparing nitride aluminum/graphite laminated composite ceramic material
CN102674903A (en) Preparation method of SiC/C-AlPO4-mullite antioxidation coating for C/C composite material
Li et al. Sealing role of Ti-rich phase in HfC-ZrC-TiC coating for C/C composites during ablation above 2100° C
RU92012719A (en) METHOD OF OBTAINING PROTECTIVE COATINGS ON MATERIALS AND PRODUCTS WITH A CARBON-CONTAINING BASE
RU2471751C1 (en) Method of producing protective coating and composition of protective coating mixture
CN1865350A (en) Organic-inorganic hybridized nano composite material resisting atomic oxygen denudation and its preparation method
CN107522508A (en) A kind of compound anti-oxidation coating and preparation method thereof
CN114315390B (en) Carbon/carbon composite material surface wide-temperature-range long-life antioxidation coating and low-temperature preparation method
CN115636692A (en) High-temperature-resistant and anti-oxidation ceramic coating and preparation method and application thereof
CN108817387A (en) A kind of preparation method of the tungsten-based composite material with high rigidity and high temperature oxidation resistance
CN105601341B (en) A method of it is prepared with beta silicon carbide coating brake disc
CN108218427B (en) Ablation-resistant ternary alloy powder consumption agent for carbon-based dissipation heat-proof composite material and method
CN107986790B (en) Antioxidant HfC/SiC foam and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication

Application publication date: 20191115

WW01 Invention patent application withdrawn after publication