CN112409005A - Preparation method of net-size C/SiC ceramic matrix composite - Google Patents

Preparation method of net-size C/SiC ceramic matrix composite Download PDF

Info

Publication number
CN112409005A
CN112409005A CN202011322374.7A CN202011322374A CN112409005A CN 112409005 A CN112409005 A CN 112409005A CN 202011322374 A CN202011322374 A CN 202011322374A CN 112409005 A CN112409005 A CN 112409005A
Authority
CN
China
Prior art keywords
carbon
composite material
zrb
zrc
sic ceramic
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.)
Granted
Application number
CN202011322374.7A
Other languages
Chinese (zh)
Other versions
CN112409005B (en
Inventor
杨良伟
霍鹏飞
刘俊鹏
宋环君
李晓东
刘伟
于新民
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.)
Aerospace Research Institute of Materials and Processing Technology
Original Assignee
Aerospace Research Institute of Materials and Processing Technology
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 Aerospace Research Institute of Materials and Processing Technology filed Critical Aerospace Research Institute of Materials and Processing Technology
Priority to CN202011322374.7A priority Critical patent/CN112409005B/en
Publication of CN112409005A publication Critical patent/CN112409005A/en
Application granted granted Critical
Publication of CN112409005B publication Critical patent/CN112409005B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

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
    • C04B35/622—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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. graphite

Abstract

The invention relates to a preparation method of a net-size C/SiC ceramic matrix composite. The preparation method comprises the following steps: (1) providing a carbon/carbon substrate; (2) carrying out ultrasonic drying and cleaning treatment on the carbon/carbon matrix, and carrying out ZrC-ZrB2Spraying a spraying agent on the surface of the carbon/carbon matrix to obtain a porous carbon/carbon composite material; (3) and (2) taking silicon alloy as a reactant, and preparing the porous carbon/carbon composite material into a net-size C/SiC ceramic matrix composite material by adopting a reaction infiltration method. The preparation method utilizes ZrC and ZrB2The silicon-based composite material has the characteristic of larger difference with the thermal expansion coefficient of silicon, so that the silicon remained and accumulated on the surface of the material presents a loose porous structure, and the net-shaped C/SiC ceramic-based composite material can be obtained by simple grinding, thereby reducing subsequent machining, effectively reducing the cost and solving the problem of preparing the C/SiC ceramic-based composite material by the traditional reaction infiltration methodThe problem of more residual alloy on the surface of the C/SiC ceramic matrix composite material.

Description

Preparation method of net-size C/SiC ceramic matrix composite
Technical Field
The invention relates to the technical field of preparation of ceramic matrix composites, in particular to a preparation method of a net-size C/SiC ceramic matrix composite.
Background
The C/SiC ceramic matrix composite material is a ceramic matrix composite material of a carbon fiber reinforced silicon carbide matrix, has the advantages of light weight, oxidation resistance, ablation resistance, corrosion resistance, high modulus and the like, can be used as a high temperature resistant structure, friction resistance and other materials, and is widely applied to the fields of aerospace, high-performance brake systems and the like.
With the rapid development of high-speed trains represented by high-speed rails, the requirements on the performance of brake friction materials such as train brake pads and the like are higher and higher, and the C/C composite material is a cast iron excellent steering performance gradually from heavy, easy-to-rust, short in service life, large in noise and poor in performance, but the C/C composite material also has the problems of high cost, long production period and the like. C/SiC ceramic matrix composites, by virtue of a low density (< 2.0 g/cm)3) The composite material has the characteristics of friction resistance, low noise, no spark, low cost and the like, can meet the requirements of high-speed trains, high-performance sports cars, heavy trucks, airplanes and the like on safety braking, and starts to carry out system intensive research on the C/SiC ceramic matrix composite material from 20 th century 90 s in various countries. German researchers try to make C/SiC ceramic matrix composite materials into automobile brake discs, apply the C/SiC ceramic matrix composite materials to high-performance Porsche automobiles for the first time, and then obtain small-range application on Racing cars such as Faraday and the like. The brake pad made of the C/SiC ceramic matrix composite material is also applied to a brake system of a high-speed train in a Japan new trunk line.
The reaction infiltration method is a method for forming a ceramic matrix composite material by reacting a high-temperature alloy with a matrix. The C/SiC ceramic matrix composite material is developed by a reaction infiltration method, and has the advantages of low cost, short preparation period and the like. However, the surface of the C/SiC ceramic matrix composite material prepared by the method often has residual silicon (figure 1) and high hardness, and the surface must be flattened by mechanical processing, so that the preparation period is prolonged, and the production cost is increased.
In order to fully exert the advantages of a reaction infiltration method in the preparation of the C/SiC ceramic matrix composite and ensure the advantages of the reaction infiltration method in the field of low-cost and high-performance brake discs, the problem of alloy residue on the surface of the C/SiC ceramic matrix composite existing in the existing reaction infiltration process needs to be solved urgently.
Disclosure of Invention
Technical problem to be solved
The invention aims to solve the technical problems that the surface of the C/SiC ceramic matrix composite prepared by the existing reaction infiltration process has alloy residues, so that the composite has higher hardness, and the composite needs to be machined and flattened, so that the preparation period is prolonged, and the production cost is increased.
(II) technical scheme
In order to solve the technical problem, the invention provides a preparation method of a net-size C/SiC ceramic matrix composite, which comprises the following steps:
(1) providing a carbon/carbon substrate;
(2) carrying out ultrasonic drying and cleaning treatment on the carbon/carbon matrix, and carrying out ZrC-ZrB2Spraying a spraying agent on the surface of the carbon/carbon matrix to obtain a porous carbon/carbon composite material;
(3) and (2) taking silicon alloy as a reactant, and preparing the porous carbon/carbon composite material into a net-size C/SiC ceramic matrix composite material by adopting a reaction infiltration method.
(III) advantageous effects
The technical scheme of the invention has the following advantages:
the invention cleans the surface of carbon/carbon matrix to prepare ZrC-ZrB2The spraying agent is prepared by controlling the concentration and the spraying time to adjust ZrC-ZrB2Thickness of coating layer, after infiltration, using ZrC, ZrB2The silicon has the characteristic of larger difference with the thermal expansion coefficient of silicon, so that the silicon remained and accumulated on the surface of the material presents a loose porous structure, the residual alloy on the surface of the composite material can be effectively reduced, and the silicon is beaten by simple sand paperAnd grinding to obtain the net-size C/SiC ceramic matrix composite, thereby effectively shortening the preparation period, reducing the preparation cost and reducing the machining process.
Drawings
The drawings of the present invention are provided for illustrative purposes only, and the scale and size in the drawings are not necessarily consistent with those of actual products.
FIG. 1 shows a ZrC-ZrB unswitched version of the present invention2And treating the C/SiC ceramic matrix composite material by using the spraying agent.
FIG. 2 shows the result of annealing in example 1, which was ZrC-ZrB2And treating the C/SiC ceramic matrix composite material by using the spraying agent.
FIG. 3 shows ZrC-ZrB arranged in example 12A spray coating agent.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a preparation method of a net-size C/SiC ceramic matrix composite, which comprises the following steps:
(1) providing a carbon/carbon substrate;
(2) carrying out ultrasonic drying and cleaning treatment on the carbon/carbon substrate to remove impurities on the surface of the substrate; and ZrC-ZrB2Spraying a spraying agent on the surface of the carbon/carbon matrix to obtain a porous carbon/carbon composite material;
(3) and (2) taking silicon alloy as a reactant, and preparing the porous carbon/carbon composite material into a net-size C/SiC ceramic matrix composite material by adopting a reaction infiltration method.
According to some preferred embodiments, the carbon/carbon matrix is prepared from a carbon fiber preform by chemical vapor deposition or other densification processes;
preferably, the preform may be knitted by any one of needle punching, sewing, fine knitting, and the like;
more preferably, the density of the carbon/carbon matrix is 1.0 to 1.4g/cm3. The limited density is 1.0-1.4g/cm3In order to subsequently make it easier to introduce the silicon alloy into the pores. The inventor finds that the density is too high, the silicon alloy is difficult to enter the material, the final content of silicon carbide is low, and the performance can not meet the requirements; if the density is too low, the silicon alloy may react with the carbon fibers, causing damage to the carbon fibers and resulting poor performance of the resulting composite.
According to some preferred embodiments, in the step (2), the ultrasonic drying and cleaning treatment is performed in the following manner: placing the carbon/carbon matrix in a beaker filled with ethanol solution, immersing, ultrasonically treating for 5-60min, then placing in an oven, and drying at 80-150 ℃.
According to some preferred embodiments, in step (2), the ZrC-ZrB2The preparation method of the spraying agent comprises the following steps:
(I) mixing ZrC powder with ZrB2Uniformly mixing the powder in an ethanol solution to obtain a colloidal solution;
(II) sequentially carrying out mechanical stirring and ultrasonic treatment on the colloidal solution to prepare the ZrC-ZrB2A spray coating agent; it is noted that ZrC-ZrB2The ethanol colloidal solution is easy to settle and needs to be prepared for use.
Preferably, the ZrC and ZrB2The powder particle size is independently 1-1000 nm;
the ZrC and the ZrB2The mass ratio of the powder is 3:1-1: 3;
the ZrC-ZrB being based on the volume of ethanol used2The total concentration of the spraying agent is 10-500% (w/v).
According to some preferred embodiments, in step (2), the ZrC-ZrB2The spraying agent is sprayed on the surface of the carbon/carbon substrate to form a coating layer with a thickness of 1-200 μm. The inventor of the invention discovers through research that ZrC-ZrB can be used2The concentration of the spraying agent and the spraying time control the thickness of the coating layer; the higher the concentration of the spraying agent, the time of sprayingThe longer the interval, the greater the thickness.
According to some preferred embodiments, in step (3), the reaction infiltration method comprises the following steps:
(I) mixing silicon alloy powder and a porous carbon/carbon composite material in a crucible;
(II) placing the crucible loaded with the silicon-zirconium alloy powder and the porous carbon/carbon composite material in a reaction device, sealing, vacuumizing, and introducing inert gas;
(III) heating the reaction device to a first preset temperature, keeping the temperature constant, heating to a second preset temperature, and keeping the temperature until the reaction is finished;
(IV) after the reaction at the second preset temperature is finished, carrying out program control cooling, cooling to room temperature, closing the inert gas, and recovering to the atmospheric pressure.
The reaction infiltration method is that the surface is coated with ZrC-ZrB under the conditions of temperature higher than the melting point of the silicon alloy and vacuum2The carbon/carbon composite material of the layer and the silicon alloy powder are subjected to in-situ reaction to obtain the ceramic matrix composite material taking silicon carbide as a matrix. The process parameters can be determined according to specific requirements in the experimental process.
In the reaction infiltration process, the surface of the composite material is coated with ZrC-ZrB with a certain thickness2Layer of ZrC, ZrB2And SiC had room temperature thermal expansion coefficients of 6.7X 10, respectively-6/K、5.6×10-6K and 2.98X 10-6The residue on the surface of the composite material is ZrC and ZrB2And the mixture of the carbon fiber and SiC has a larger thermal expansion coefficient, so that surface residues can present a loose and porous structure, the bonding force with the surface of a matrix is weaker, the surface residues can be removed by simply processing with sand paper, and finally the net-size C/SiC ceramic matrix composite is obtained.
According to some preferred embodiments, the mass ratio of the porous carbon/carbon composite to the silicon alloy is 1:3 to 1: 6; the inventor finds that if the addition amount of the silicon alloy powder is too much, the silicon alloy powder is not beneficial to the uniform dispersion of the alloy powder; if the addition amount of the silicon alloy powder is too small, the alloy proportion in the carbon matrix is low, and the uniformity and the performance of the subsequent matrix are greatly influenced. Under the same condition, in the range, the higher the proportion of the silicon alloy powder is, the higher the SiC content in the final product is, the more uniform the matrix distribution is, and the stronger the performance is.
The silicon alloy powder is a commercial product and is purchased from the Limited liability company of the Jinfeng silicon product in Jinan; preferably, the silicon alloy has a particle size of 0.5 to 10 μm;
more preferably, the silicon alloy has a silicon mass fraction of 95 to 99%.
According to some preferred embodiments, the introduced inert gas is argon or nitrogen;
the flow rate of the introduced inert gas is 1-1000 sccm.
According to some preferred embodiments, the first preset temperature is 1200-;
the second preset temperature is 1600-1700 ℃, and the reaction is carried out for 1-180 minutes at the second preset temperature;
the heating rate of heating to the first preset temperature and the heating rate of heating to the second preset temperature are independently 1-40 ℃/min;
according to some preferred embodiments, the programmed controlled cooling rate is 1-40 ℃/min.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified. All percentages and parts are by weight unless otherwise indicated.
Example 1
(1) Providing a carbon/carbon matrix: preparing carbon/carbon matrix from carbon fiber preform by chemical vapor deposition method, and selecting density of 1.1g/cm3The carbon/carbon substrate of (2), wherein the carbon fiber preform is woven in a needle-punched manner;
(2) carrying out ultrasonic drying and cleaning treatment on the carbon/carbon matrix: placing the carbon/carbon matrix in an ethanol solution, completely immersing, performing ultrasonic treatment for 30min, and then placing in an oven to perform drying treatment at 80 ℃;
(3)ZrC-ZrB2spraying of paintPreparation of the agent: ZrC and ZrB2The particle size of the powder is 100nm, the mass ratio of the powder to the powder is 3:1, the powder and the powder are added into ethanol and evenly mixed to obtain a colloidal solution, and the total concentration ratio is 100% (g/mL). Sequentially carrying out mechanical stirring and ultrasonic treatment on the colloidal solution to finally obtain uniformly dispersed ZrC-ZrB2Spray coating agent (fig. 3);
(4) coating ZrC-ZrB2Layer (b): ZrC-ZrB2Spraying the carbon/carbon matrix subjected to surface ultrasonic drying and cleaning treatment with a spraying agent for 5min, wherein the thickness is about 50 μm, and standing to obtain a porous carbon/carbon composite material;
(5) and (3) reaction infiltration treatment: coating ZrC-ZrB on the surface2The porous carbon/carbon composite material of the layer is placed in a graphite crucible and is mixed with silicon alloy powder according to the mass ratio of 1:3, wherein the particle size of the silicon alloy powder is 5 mu m, and the mass fraction of silicon is 95%. Placing the crucible in a high-temperature furnace body, vacuumizing, introducing argon gas with the flow rate of 1000sccm, heating the reaction device to 1200 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 200min at constant temperature, heating to 1600 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 100min until the reaction is finished; after the reaction, the reaction mixture was cooled to room temperature at a cooling rate of 10 ℃/min, the introduction of the inert gas was stopped, and the pressure was returned to atmospheric pressure. And (3) obtaining the net-size C/SiC ceramic matrix composite material by simple sand paper grinding, wherein the surface of the material is clean (figure 2).
Example 2
(1) Providing a carbon/carbon matrix: preparing carbon/carbon matrix from carbon fiber preform by chemical vapor deposition method, and selecting density of 1.1g/cm3The carbon/carbon substrate of (2), wherein the carbon fiber preform is woven in a needle-punched manner;
(2) carrying out ultrasonic drying and cleaning treatment on the carbon/carbon matrix: placing the carbon/carbon matrix in an ethanol solution, completely immersing, carrying out ultrasonic treatment for 30min, and then placing in an oven for drying treatment at 100 ℃;
(3)ZrC-ZrB2preparing a spraying agent: ZrC and ZrB2The powder particle diameter is 100nm, the mass ratio of the powder particle diameter to the powder particle diameter is 2:1, the powder particle diameter and the powder particle diameter are added into ethanol and uniformly mixed to obtain colloidal solution, and the total weight of the colloidal solution isThe concentration ratio was 150% (g/mL). Sequentially carrying out mechanical stirring and ultrasonic treatment on the colloidal solution to finally obtain uniformly dispersed ZrC-ZrB2Ethanol colloidal solution;
(4) coating ZrC-ZrB2Layer (b): ZrC-ZrB2Spraying the carbon/carbon matrix subjected to surface ultrasonic drying and cleaning treatment with a spraying agent for 5min, wherein the thickness is about 70 mu m, and standing to obtain the porous carbon/carbon composite material;
(5) and (3) reaction infiltration treatment: coating ZrC-ZrB on the surface2The porous carbon/carbon composite material of the layer is placed in a graphite crucible and is mixed with silicon alloy powder according to the mass ratio of 1:3, wherein the particle size of the silicon alloy powder is 5 mu m, and the mass fraction of silicon is 95%. Placing the crucible in a high-temperature furnace body, vacuumizing, introducing argon gas with the flow rate of 1000sccm, heating the reaction device to 1260 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 180min at constant temperature, heating to 1680 ℃ at the heating rate of 10 ℃/min, and keeping the temperature for 140min until the reaction is finished; after the reaction, the reaction mixture was cooled to room temperature at a cooling rate of 10 ℃/min, the introduction of the inert gas was stopped, and the pressure was returned to atmospheric pressure. And (3) obtaining the net-size C/SiC ceramic matrix composite material by simple sand paper polishing, wherein the surface of the material is clean.
Example 3
This example 3 is substantially the same as example 2 except that: ZrC and ZrB2The mass ratio of the powder is 1:1, the total concentration ratio is 200% (g/mL), ZrC-ZrB2The layer thickness was 100 μm.
And (3) obtaining the net-size C/SiC ceramic matrix composite material by simple sand paper polishing, wherein the surface of the material is clean.
Example 4
This example 4 is substantially the same as example 2 except that:
the density of the porous carbon/carbon composite material is 1.2g/cm3ZrC and ZrB2The mass ratio of the powder is 3:1, the total concentration ratio is 100 percent (g/mL), ZrC-ZrB2The layer thickness was 50 μm.
And (3) obtaining the net-size C/SiC ceramic matrix composite material by simple sand paper polishing, wherein the surface of the material is clean.
Example 5
This example 5 is substantially the same as example 2 except that: the density of the porous carbon/carbon composite material is 1.2g/cm3ZrC and ZrB2The mass ratio of the powder is 2:1, the total concentration ratio is 300 percent (g/mL), ZrC-ZrB2The layer thickness was 100 μm.
And (3) obtaining the net-size C/SiC ceramic matrix composite material by simple sand paper polishing, wherein the surface of the material is clean.
Example 6
This example 6 is substantially the same as example 2 except that: the density of the porous carbon/carbon composite material is 1.3g/cm3ZrC and ZrB2The mass ratio of the powder is 1:1, the total concentration ratio is 200% (g/mL), ZrC-ZrB2The layer thickness was 50 μm.
And (3) obtaining the net-size C/SiC ceramic matrix composite material by simple sand paper polishing, wherein the surface of the material is clean.
TABLE 1 Process parameters for the examples and resulting composite surface cleanliness
Figure BDA0002793334810000091
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A preparation method of net-size C/SiC ceramic matrix composite is characterized by comprising the following steps:
(1) providing a carbon/carbon substrate;
(2) carrying out ultrasonic drying and cleaning treatment on the carbon/carbon matrix, and carrying out ZrC-ZrB2Spraying a spraying agent on the surface of the carbon/carbon matrix to obtain a porous carbon/carbon composite material;
(3) and (2) taking silicon alloy as a reactant, and preparing the porous carbon/carbon composite material into a net-size C/SiC ceramic matrix composite material by adopting a reaction infiltration method.
2. The method of claim 1, wherein:
the carbon/carbon matrix is prepared from a carbon fiber preform by a chemical vapor deposition method;
preferably, the preform is woven in a manner selected from the group consisting of needling, stitching, or fine knitting;
more preferably, the carbon/carbon matrix has a density of 1.0 to 1.4g/cm3。
3. The method of claim 1, wherein:
in the step (2), the ultrasonic drying and cleaning treatment mode is as follows: and (2) placing the carbon/carbon matrix in a beaker filled with ethanol solution, immersing, carrying out ultrasonic treatment for 5-60min, then placing in an oven, and carrying out drying treatment at 80-150 ℃.
4. The method of claim 1, wherein:
in the step (2), the ZrC-ZrB2The preparation method of the spraying agent comprises the following steps:
(I) mixing ZrC powder with ZrB2Uniformly mixing the powder in an ethanol solution to obtain a colloidal solution;
(II) sequentially carrying out mechanical stirring and ultrasonic treatment on the colloidal solution to prepare the ZrC-ZrB2A spray coating agent;
preferably, the ZrC and ZrB2The powder particle size is independently 1-1000 nm;
the ZrC and the ZrB2The mass ratio of the powder is 3:1-1: 3;
the ZrC-ZrB being based on the volume of ethanol used2The total concentration of the spraying agent is 10-500% (w/v).
5. The method of claim 1, wherein:
in the step (2), the ZrC-ZrB2The thickness of the coating layer sprayed on the surface of the carbon/carbon matrix by the spraying agent is 1-200 mu m;
the spraying time is 5-10 min.
6. The method of claim 1, wherein:
in the step (3), the reaction infiltration method comprises the following steps:
(I) mixing silicon alloy powder and a porous carbon/carbon composite material in a crucible;
(II) placing the crucible loaded with the silicon alloy powder and the porous carbon/carbon composite material in a reaction device, sealing, vacuumizing, and introducing inert gas;
(III) heating the reaction device to a first preset temperature, keeping the temperature constant, heating to a second preset temperature, and keeping the temperature until the reaction is finished;
(IV) after the reaction at the second preset temperature is finished, carrying out program control cooling, cooling to room temperature, stopping introducing the inert gas, and recovering to the atmospheric pressure.
7. The method of claim 6, wherein:
the mass ratio of the porous carbon/carbon composite material to the silicon alloy is 1:3-1: 6;
preferably, the silicon alloy has a particle size of 0.5 to 10 μm;
more preferably, the silicon alloy has a silicon mass fraction of 95 to 99%.
8. The production method according to claim 6 or 7, characterized in that:
the introduced inert gas is argon or nitrogen;
the flow rate of the introduced gas is 1-1000 sccm.
9. The production method according to any one of claims 6 to 8, characterized in that:
the first preset temperature is 1200-1400 ℃, and the constant temperature is kept for 1-200 minutes at the first preset temperature;
the second preset temperature is 1600-1700 ℃, and the reaction is carried out for 1-180 minutes at the second preset temperature;
the heating rate for heating to the first preset temperature and the heating rate for heating to the second preset temperature are independently 1-40 ℃/min.
10. The production method according to any one of claims 6 to 9, characterized in that:
the program controls the cooling rate of the cooling to be 1-40 ℃/min.
CN202011322374.7A 2020-11-23 2020-11-23 Preparation method of net-size C/SiC ceramic matrix composite Active CN112409005B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011322374.7A CN112409005B (en) 2020-11-23 2020-11-23 Preparation method of net-size C/SiC ceramic matrix composite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011322374.7A CN112409005B (en) 2020-11-23 2020-11-23 Preparation method of net-size C/SiC ceramic matrix composite

Publications (2)

Publication Number Publication Date
CN112409005A true CN112409005A (en) 2021-02-26
CN112409005B CN112409005B (en) 2022-03-29

Family

ID=74777897

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011322374.7A Active CN112409005B (en) 2020-11-23 2020-11-23 Preparation method of net-size C/SiC ceramic matrix composite

Country Status (1)

Country Link
CN (1) CN112409005B (en)

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100061847A1 (en) * 2008-09-09 2010-03-11 General Electric Company Steam turbine part including ceramic matrix composite (cmc)
CN103113124A (en) * 2013-02-04 2013-05-22 西安交通大学 Preparation method of fiber-toughened SiC ceramic-based composite material three-dimensional member
US20130167374A1 (en) * 2011-12-29 2013-07-04 General Electric Company Process of producing ceramic matrix composites and ceramic matrix composites formed thereby
CN103724031A (en) * 2013-05-28 2014-04-16 太仓派欧技术咨询服务有限公司 Ceramic matrix composite material applied to high-speed motor car brake disc and preparation method thereof
CN107540411A (en) * 2017-08-22 2018-01-05 巩义市泛锐熠辉复合材料有限公司 It is a kind of to reduce the method that silicone content is remained in carbon fibre reinforced ceramics based composites
CN108191447A (en) * 2018-01-17 2018-06-22 长沙理工大学 A kind of preparation method of the anti-oxidant C/C-ZrC of resistance to ablation carbon ceramic composite material
US20180194690A1 (en) * 2017-01-11 2018-07-12 General Electric Company Carbon yielding resin for melt infiltration
CN108503390A (en) * 2018-05-04 2018-09-07 西北工业大学 Surface of carbon/carbon composite inlays SiC-ZrB2-ZrSi2The preparation method of compound anti-oxidation coating
CN110256093A (en) * 2019-07-09 2019-09-20 中国航发北京航空材料研究院 A kind of reduction infiltration process preparation SiCfThe method of remaining silicone content in/SiC ceramic matrix composite material
CN110563479A (en) * 2019-10-25 2019-12-13 航天特种材料及工艺技术研究所 Ultrahigh-temperature ceramic matrix composite and preparation method thereof

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100061847A1 (en) * 2008-09-09 2010-03-11 General Electric Company Steam turbine part including ceramic matrix composite (cmc)
US20130167374A1 (en) * 2011-12-29 2013-07-04 General Electric Company Process of producing ceramic matrix composites and ceramic matrix composites formed thereby
CN103113124A (en) * 2013-02-04 2013-05-22 西安交通大学 Preparation method of fiber-toughened SiC ceramic-based composite material three-dimensional member
CN103724031A (en) * 2013-05-28 2014-04-16 太仓派欧技术咨询服务有限公司 Ceramic matrix composite material applied to high-speed motor car brake disc and preparation method thereof
US20180194690A1 (en) * 2017-01-11 2018-07-12 General Electric Company Carbon yielding resin for melt infiltration
CN107540411A (en) * 2017-08-22 2018-01-05 巩义市泛锐熠辉复合材料有限公司 It is a kind of to reduce the method that silicone content is remained in carbon fibre reinforced ceramics based composites
CN108191447A (en) * 2018-01-17 2018-06-22 长沙理工大学 A kind of preparation method of the anti-oxidant C/C-ZrC of resistance to ablation carbon ceramic composite material
CN108503390A (en) * 2018-05-04 2018-09-07 西北工业大学 Surface of carbon/carbon composite inlays SiC-ZrB2-ZrSi2The preparation method of compound anti-oxidation coating
CN110256093A (en) * 2019-07-09 2019-09-20 中国航发北京航空材料研究院 A kind of reduction infiltration process preparation SiCfThe method of remaining silicone content in/SiC ceramic matrix composite material
CN110563479A (en) * 2019-10-25 2019-12-13 航天特种材料及工艺技术研究所 Ultrahigh-temperature ceramic matrix composite and preparation method thereof

Also Published As

Publication number Publication date
CN112409005B (en) 2022-03-29

Similar Documents

Publication Publication Date Title
RU2176628C2 (en) Composite material (variants) and method or preparing thereof, method of treating fibrous semi-finished product (variants)
JP4974209B2 (en) Silicon infiltration treatment method for ceramic matrix composites
CN110668838B (en) Carbon-ceramic brake component and preparation method thereof
CN109251052B (en) C/C composite material and preparation method thereof
CN101544851B (en) Metallic bond hollow sphere-shaped super-hard compound material and manufacturing method thereof
CN105565837B (en) A kind of preparation method and applications of carbon ceramic composite material
CN108264368B (en) Carbon-ceramic composite material with self-lubricating and anti-oxidation functions and preparation method thereof
CN110937910B (en) Preparation method of composite nano refractory ceramic modified carbon/carbon composite material
CN106478125A (en) A kind of B4The preparation method of C modification C/C SiC brake material
CN110683853B (en) Preparation method of silicon nitride and silicon carbide combined friction material
CN110372408B (en) Ceramic fiber toughened CVD silicon carbide composite material and preparation method and application thereof
CN109942317A (en) Surface of carbon/carbon composite mullite crystal whisker-mullite/yttrium aluminosilicate compound anti-oxidation coating and preparation method
CN113045326B (en) Preparation method of modified carbon/carbon composite material
IL134576A (en) Method for producing abrasive grains and the abrasive grains produced by this method
CN115677370A (en) Preparation method of carbon-ceramic brake material
CN109704798A (en) The method that vacuum impregnation association reaction melt infiltration RMI prepares C/SiC-Diamond composite material
CN104313518A (en) Ceramic composite material as well as preparation method and application thereof
CN108727049B (en) CfSiC-HfC ultrahigh-temperature ceramic matrix composite and preparation method thereof
CN105350294A (en) Silicon carbide layer coated short carbon fiber and preparation method thereof
CN112409005B (en) Preparation method of net-size C/SiC ceramic matrix composite
Camarano et al. Effects of Fe addition on the mechanical and thermo-mechanical properties of SiC/FeSi2/Si composites produced via reactive infiltration
JP2010516981A (en) Brake disc and clutch disc improvements or related improvements
CN112374906A (en) Preparation method of carbon fiber toughened silicon carbide-zirconium carbide composite material
CN112830805A (en) Preparation method of carbon-ceramic wear-resistant composite material
CN115773321A (en) High strength charcoal/pottery brake disc with pottery functional layer

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
GR01 Patent grant
GR01 Patent grant