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CN109987955A - A kind of C effectively improving interfacial combined functionf/ SiC ceramic matrix composite material and preparation method - Google Patents

A kind of C effectively improving interfacial combined functionf/ SiC ceramic matrix composite material and preparation method Download PDF

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CN109987955A
CN109987955A CN201910292816.9A CN201910292816A CN109987955A CN 109987955 A CN109987955 A CN 109987955A CN 201910292816 A CN201910292816 A CN 201910292816A CN 109987955 A CN109987955 A CN 109987955A
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王小玲
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/565Shaped 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
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/524Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248Carbon, e.g. graphite

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  • Ceramic Engineering (AREA)
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Abstract

The present invention relates to Ceramic Matrix Composites Reinforced by Carbon Fibers technical fields, and disclose a kind of C for effectively improving interfacial combined functionf/ SiC ceramic matrix composite material, the raw material including following parts by weight proportion: 50~70 parts of micron SiC ceramic powders, 10~20 parts of micron CfPowder, 5~10 parts of Nano-meter SiO_2s2Powder, 8~15 powder micrometer ceramics binders.The invention also discloses a kind of C for effectively improving interfacial combined functionfThe preparation method of/SiC ceramic matrix composite material.The present invention solves Cf/ SiC ceramic matrix composite material, during the preparation process, since carbon fiber surface shows lyophobicity, the technical problem of boundary moisture performance difference between caused carbon fiber and silicon carbide substrate.

Description

A kind of C effectively improving interfacial combined functionf/ SiC ceramic matrix composite material and preparation method
Technical field
The present invention relates to Ceramic Matrix Composites Reinforced by Carbon Fibers technical field, specially one kind effectively improves boundary The C of face binding performancef/ SiC ceramic matrix composite material and preparation method.
Background technique
Silicon carbide ceramics because have high intensity, high rigidity, anticorrosive, high temperature resistant and low-density due to be widely used in high temperature and In certain harsh environments, especially there is very big dive in the privileged sites that aerospace flight vehicle needs to bear excessive temperature Power.But ceramics do not have the plastic deformation ability as metal, inhale in fracture process in addition to generating new break surface It receives other than the energy of surface, almost without other mechanism for absorbing energy, this just seriously limits its application as structural material.
Carbon fiber has many advantages, such as that specific strength is high, specific modulus is big, mechanical behavior under high temperature and hot property are good, in inert atmosphere In 2000 DEG C when be still able to maintain rheobase and originally do not decline.With carbon fibre reinforced silicon carbide composite material, process of the material in fracture In by toughening mechanisms such as spike protein gene, fiber-bridged, crack deflections consume energy, so that material is shown as non-brittle fracture. Cf/ SiC ceramic matrix composite material combines the excellent high-temperature behavior of carbon fiber and silicon carbide substrate high antioxygenic property, receives height and closes Note, and it is widely used in aerospace field.
But in preparation CfDuring/SiC ceramic matrix composite material, since the specific surface area active of carbon fiber is small (generally less than 1m2/ g), surface can be low, and surface shows lyophobicity, so that there is interfacial wettabilities between carbon fiber and silicon carbide substrate is poor The problem of.
In order to improve the chemical mobility of the surface of carbon fiber, enhance the binding ability of carbon fiber surface and silicon carbide substrate, into And the performance of composite material is improved, it is necessary for carrying out surface treatment to carbon fiber.Currently, carbon fiber surface modification is handled Mainly there are the methods of surface oxidation treatment, surface coated treatment, surface growth whisker.But single surface treatment is usually mentioning While certain high aspect performance, the performance of another aspect is sacrificed, and compound base amount method rule can be used by just compromise The advantages of several surface treatment methods, will become the main direction of studying of surface treatment of carbon fibers from now on.
The present invention provides a kind of C for effectively improving interfacial combined functionf/ SiC ceramic matrix composite material and preparation method, it is intended to solve Cf/ SiC ceramic matrix composite material, during the preparation process, since carbon fiber surface shows lyophobicity, caused carbon fiber and silicon carbide The technical problem of boundary moisture performance difference between matrix.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of C for effectively improving interfacial combined functionf/ SiC composite wood Material and preparation method, solve Cf/ SiC ceramic matrix composite material, during the preparation process, since carbon fiber surface shows lyophobicity, institute The technical problem of boundary moisture performance difference between caused carbon fiber and silicon carbide substrate.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
A kind of C effectively improving interfacial combined functionf/ SiC ceramic matrix composite material, the raw material including following parts by weight proportion: 50~70 parts of micron SiC ceramic powders, 10~20 parts of micron CfPowder, 5~10 parts of Nano-meter SiO_2s2Powder, 8~15 powder micrometer ceramics bonding Agent.
Preferably, the Nano-meter SiO_22Average grain diameter≤100nm of powder.
Preferably, the vitrified bonding is by average grain diameter≤2.6um 30%wtSiO2, 30%wt Al2O3, 25%wt ZrO2And 15%wtTiO2Composition.
A kind of C effectively improving interfacial combined functionfThe preparation method of/SiC ceramic matrix composite material, comprising the following steps:
S101. 50~70 parts of micron SiC ceramic powders, 10~20 parts of micron C are takenfPowder, 5~10 parts of Nano-meter SiO_2s2Powder, 8~15 Powder micrometer ceramics binder, it is spare;
S102. the SiC powder in step S101 is placed in distilled water together with sodium metasilicate, ultrasonic disperse is uniform;
S103. by the C in step S101fPowder particles are placed in distilled water together with sodium pyrophosphate, and ultrasonic disperse is uniform;
S104. by the SiO in step S1012Powder is placed in distilled water together with sodium metasilicate, and ultrasonic disperse is uniform;
S105. the SiC dispersion liquid in step S102 is added in the reactor equipped with agitating device and heating device, Under the stirring rate of 600r/min, slowly by the C in step S103fDispersant liquid drop is added in reactor, after being added dropwise, slowly By the SiO in step S1042Dispersant liquid drop is added in reactor, and after being added dropwise, 2h is stirred under 800r/min, later, Under 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed;
S106. the vitrified bonding in step S101 is added to reacting equipped with blender with the powder in step S105 In device, at 800r/min, 2h is stirred;
S107. the powder in step S106 is fitted into etc. in static pressure rubber mold, the compression moulding under 600MPa pressure, is risen Temperature keeps the temperature 3h to 2800 DEG C, and under 2800 DEG C, 15MPa, and C is preparedf/ SiC ceramic matrix composite material.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
The present invention is in matrix SiC ceramic phase and reinforced phase CfIncrease vitrified bonding and adhesive aid Nano-meter SiO_2 between powder2 Powder, vitrified bonding and adhesive aid Nano-meter SiO_22Powder can effectively improve matrix SiC ceramic phase and reinforced phase CfBetween powder Wettability, to improve matrix SiC ceramic phase and reinforced phase CfAdhesive property between powder;
C prepared by the present inventionf/ SiC ceramic matrix composite material, tensile strength is 167~180MPa, stretch modulus be 79~ 83GPa, bending strength are 294~316MPa, bending modulus is 78~89GPa;
With the C in comparative examplefTensile strength 160MPa, the stretch modulus 65GPa, bending strength of/SiC ceramic matrix composite material 288MPa, bending modulus 68GPa are compared, and are achieved and are significantly improved CfThe technical effect of the mechanical property of/SiC ceramic matrix composite material.
Specific embodiment
Embodiment one:
Above-mentioned CfThe preparation method of/SiC ceramic matrix composite material the following steps are included:
S101. 50g average particle size≤25um SiC ceramic powder, 20g average grain diameter≤10um C are takenfPowder, 5g are averaged grain Diameter≤100nm SiO2Powder, 15g average grain diameter≤2.6um vitrified bonding, it is spare;Wherein, vitrified bonding is by 30% wtSiO2, 30%wt Al2O3, 25%wt ZrO2And 15%wtTiO2Composition;
S102. the SiC powder in step S101 is placed in 100mL distilled water together with 5g sodium metasilicate, ultrasonic disperse is uniform;
S103. by the C in step S101fPowder particles are placed in 30mL distilled water together with 2g sodium pyrophosphate, ultrasonic disperse Uniformly;
S104. by the SiO in step S1012Powder is placed in 20mL distilled water together with 1g sodium metasilicate, and ultrasonic disperse is uniform;
S105. the SiC dispersion liquid in step S102 is added in the reactor equipped with agitating device and heating device, Under the stirring rate of 600r/min, slowly by the C in step S103fDispersant liquid drop is added in reactor, after being added dropwise, slowly By the SiO in step S1042Dispersant liquid drop is added in reactor, and after being added dropwise, 2h is stirred under 800r/min, later, Under 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed;
S106. the vitrified bonding in step S101 is added to reacting equipped with blender with the powder in step S105 In device, at 800r/min, 2h is stirred;
S107. the powder in step S106 is fitted into etc. in static pressure rubber mold, the compression moulding under 600MPa pressure, then Being placed in preheating temperature is in 1250 DEG C of vacuum drying oven, with the heating rate of 10 DEG C/min, is warming up to 2800 DEG C, and in 2800 DEG C, 3h is kept the temperature under 15MPa, later with the annealing rate of 10 DEG C/min, C is prepared in taking-up when being cooled to room temperaturef/ SiC composite wood Material.
Embodiment two:
S101. 70g average particle size≤25um SiC ceramic powder, 10g average grain diameter≤10um C are takenfPowder, 10g are averaged grain Diameter≤100nm SiO2Powder, 8g average grain diameter≤2.6um vitrified bonding, it is spare;Wherein, vitrified bonding is by 30% wtSiO2, 30%wt Al2O3, 25%wt ZrO2And 15%wtTiO2Composition;
S102. the SiC powder in step S101 is placed in 100mL distilled water together with 5g sodium metasilicate, ultrasonic disperse is uniform;
S103. by the C in step S101fPowder particles are placed in 30mL distilled water together with 2g sodium pyrophosphate, ultrasonic disperse Uniformly;
S104. by the SiO in step S1012Powder is placed in 20mL distilled water together with 1g sodium metasilicate, and ultrasonic disperse is uniform;
S105. the SiC dispersion liquid in step S102 is added in the reactor equipped with agitating device and heating device, Under the stirring rate of 600r/min, slowly by the C in step S103fDispersant liquid drop is added in reactor, after being added dropwise, slowly By the SiO in step S1042Dispersant liquid drop is added in reactor, and after being added dropwise, 2h is stirred under 800r/min, later, Under 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed;
S106. the vitrified bonding in step S101 is added to reacting equipped with blender with the powder in step S105 In device, at 800r/min, 2h is stirred;
S107. the powder in step S106 is fitted into etc. in static pressure rubber mold, the compression moulding under 600MPa pressure, then Being placed in preheating temperature is in 1250 DEG C of vacuum drying oven, with the heating rate of 10 DEG C/min, is warming up to 2800 DEG C, and in 2800 DEG C, 3h is kept the temperature under 15MPa, later with the annealing rate of 10 DEG C/min, C is prepared in taking-up when being cooled to room temperaturef/ SiC composite wood Material.
Embodiment three:
S101. 60g average particle size≤25um SiC ceramic powder, 15g average grain diameter≤10um C are takenfPowder, 8g are averaged grain Diameter≤100nm SiO2Powder, 12g average grain diameter≤2.6um vitrified bonding, it is spare;Wherein, vitrified bonding is by 30% wtSiO2, 30%wt Al2O3, 25%wt ZrO2And 15%wtTiO2Composition;
S102. the SiC powder in step S101 is placed in 100mL distilled water together with 5g sodium metasilicate, ultrasonic disperse is uniform;
S103. by the C in step S101fPowder particles are placed in 30mL distilled water together with 2g sodium pyrophosphate, ultrasonic disperse Uniformly;
S104. by the SiO in step S1012Powder is placed in 20mL distilled water together with 1g sodium metasilicate, and ultrasonic disperse is uniform;
S105. the SiC dispersion liquid in step S102 is added in the reactor equipped with agitating device and heating device, Under the stirring rate of 600r/min, slowly by the C in step S103fDispersant liquid drop is added in reactor, after being added dropwise, slowly By the SiO in step S1042Dispersant liquid drop is added in reactor, and after being added dropwise, 2h is stirred under 800r/min, later, Under 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed;
S106. the vitrified bonding in step S101 is added to reacting equipped with blender with the powder in step S105 In device, at 800r/min, 2h is stirred;
S107. the powder in step S106 is fitted into etc. in static pressure rubber mold, the compression moulding under 600MPa pressure, then Being placed in preheating temperature is in 1250 DEG C of vacuum drying oven, with the heating rate of 10 DEG C/min, is warming up to 2800 DEG C, and in 2800 DEG C, 3h is kept the temperature under 15MPa, later with the annealing rate of 10 DEG C/min, C is prepared in taking-up when being cooled to room temperaturef/ SiC composite wood Material.
Comparative example:
CfThe preparation method of/SiC ceramic matrix composite material the following steps are included:
S101. 50g average particle size≤25um SiC ceramic powder, 20g average grain diameter≤10um C are takenfIt is powder, spare;Its In, vitrified bonding is by 30%wtSiO2, 30%wt Al2O3, 25%wt ZrO2And 15%wtTiO2Composition;
S102. the SiC powder in step S101 is placed in 100mL distilled water together with 5g sodium metasilicate, ultrasonic disperse is uniform;
S103. by the C in step S101fPowder particles are placed in 30mL distilled water together with 2g sodium pyrophosphate, ultrasonic disperse Uniformly;
S104. the SiC dispersion liquid in step S102 is added in the reactor equipped with agitating device and heating device, Under the stirring rate of 600r/min, slowly by the C in step S103fDispersant liquid drop is added in reactor, after being added dropwise, in 2h is stirred under 800r/min, later, at 120 DEG C of temperature, stirring rate 300r/min, solvent is evaporated and is removed;
S105. the powder in step S104 is fitted into etc. in static pressure rubber mold, the compression moulding under 600MPa pressure, then Being placed in preheating temperature is in 1250 DEG C of vacuum drying oven, with the heating rate of 10 DEG C/min, is warming up to 2800 DEG C, and in 2800 DEG C, 3h is kept the temperature under 15MPa, later with the annealing rate of 10 DEG C/min, C is prepared in taking-up when being cooled to room temperaturef/ SiC composite wood Material.
Performance test:
To the C prepared in above-described embodiment and comparative examplef/ SiC ceramic matrix composite material is tested for the property, and performance data is as follows Shown in table 1.
Table 1

Claims (4)

1. a kind of C for effectively improving interfacial combined functionf/ SiC ceramic matrix composite material, which is characterized in that matched including following parts by weight Raw material: 50~70 parts of micron SiC ceramic powders, 10~20 parts of micron CfPowder, 5~10 parts of Nano-meter SiO_2s2Powder, 8~15 powder microns pottery Porcelain binder.
2. C according to claim 1f/ SiC ceramic matrix composite material, which is characterized in that the Nano-meter SiO_22The average grain diameter of powder≤ 100nm。
3. C according to claim 1f/ SiC ceramic matrix composite material, which is characterized in that the vitrified bonding by average grain diameter≤ The 30%wtSiO of 2.6um2, 30%wt Al2O3, 25%wt ZrO2And 15%wtTiO2Composition.
4. a kind of C for effectively improving interfacial combined functionfThe preparation method of/SiC ceramic matrix composite material, which is characterized in that including following step It is rapid:
S101. 50~70 parts of micron SiC ceramic powders, 10~20 parts of micron C are takenfPowder, 5~10 parts of Nano-meter SiO_2s2Powder, 8~15 powder are micro- Rice vitrified bonding, it is spare;
S102. the SiC powder in step S101 is placed in distilled water together with sodium metasilicate, ultrasonic disperse is uniform;
S103. by the C in step S101fPowder particles are placed in distilled water together with sodium pyrophosphate, and ultrasonic disperse is uniform;
S104. by the SiO in step S1012Powder is placed in distilled water together with sodium metasilicate, and ultrasonic disperse is uniform;
S105. the SiC dispersion liquid in step S102 is added in the reactor equipped with agitating device and heating device, in 600r/ Under the stirring rate of min, slowly by the C in step S103fDispersant liquid drop is added in reactor, slowly will step after being added dropwise SiO in rapid S1042Dispersant liquid drop is added in reactor, after being added dropwise, 2h is stirred under 800r/min, later, in temperature 120 DEG C, under stirring rate 300r/min, solvent is evaporated and is removed;
S106. the powder in the vitrified bonding and step S105 in step S101 is added to the reactor equipped with blender In, at 800r/min, stir 2h;
S107. the powder in step S106 is fitted into etc. in static pressure rubber mold, the compression moulding under 600MPa pressure is warming up to 2800 DEG C, and 3h is kept the temperature under 2800 DEG C, 15MPa, C is preparedf/ SiC ceramic matrix composite material.
CN201910292816.9A 2019-04-12 2019-04-12 A kind of C effectively improving interfacial combined functionf/ SiC ceramic matrix composite material and preparation method Withdrawn CN109987955A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114455968A (en) * 2022-02-10 2022-05-10 航天材料及工艺研究所 A kind of C/SiC-SiO2 composite material and preparation method thereof

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CN101164993A (en) * 2006-10-16 2008-04-23 宁波大学 Method for preparing silicon carbide ceramic composition containing fibre and whisker
CN101314543A (en) * 2007-06-01 2008-12-03 哈尔滨工业大学 High-quality short carbon fiber toughened silicon carbide composite material, preparation method and application
CN102295465A (en) * 2011-06-10 2011-12-28 陕西科技大学 Hot-press preparation method of short carbon fiber/silicon carbide composite material
CN104446393A (en) * 2014-12-01 2015-03-25 青岛麦特瑞欧新材料技术有限公司 Yttrium-doped inorganic nanocomposite material for 3D printing and preparation method of yttrium-doped inorganic nanocomposite material
CN104829255A (en) * 2015-04-20 2015-08-12 凤阳徽亨商贸有限公司 Ceramic silicon carbide grinding wheel containing carbon reinforced fiber
CN105690807A (en) * 2016-02-06 2016-06-22 陕西科技大学 Preparation method and application of carbon fiber reinforced polymer-based composite
CN107056315A (en) * 2016-12-16 2017-08-18 吴中区穹窿山天仲高分子材料技术研究所 A kind of silicon carbide ceramics for being embedded with plasticizing substance

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Publication number Priority date Publication date Assignee Title
JPH01104879A (en) * 1987-10-15 1989-04-21 Ibiden Co Ltd Composite carbon fiber and its production
CN101164993A (en) * 2006-10-16 2008-04-23 宁波大学 Method for preparing silicon carbide ceramic composition containing fibre and whisker
CN101314543A (en) * 2007-06-01 2008-12-03 哈尔滨工业大学 High-quality short carbon fiber toughened silicon carbide composite material, preparation method and application
CN102295465A (en) * 2011-06-10 2011-12-28 陕西科技大学 Hot-press preparation method of short carbon fiber/silicon carbide composite material
CN104446393A (en) * 2014-12-01 2015-03-25 青岛麦特瑞欧新材料技术有限公司 Yttrium-doped inorganic nanocomposite material for 3D printing and preparation method of yttrium-doped inorganic nanocomposite material
CN104829255A (en) * 2015-04-20 2015-08-12 凤阳徽亨商贸有限公司 Ceramic silicon carbide grinding wheel containing carbon reinforced fiber
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CN107056315A (en) * 2016-12-16 2017-08-18 吴中区穹窿山天仲高分子材料技术研究所 A kind of silicon carbide ceramics for being embedded with plasticizing substance

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114455968A (en) * 2022-02-10 2022-05-10 航天材料及工艺研究所 A kind of C/SiC-SiO2 composite material and preparation method thereof
CN114455968B (en) * 2022-02-10 2023-08-29 航天材料及工艺研究所 A kind of C/SiC-SiO2 composite material and preparation method thereof

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