CN112358315A - Preparation method of ceramic matrix composite material containing cooling pore channel - Google Patents

Preparation method of ceramic matrix composite material containing cooling pore channel Download PDF

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CN112358315A
CN112358315A CN202011361049.1A CN202011361049A CN112358315A CN 112358315 A CN112358315 A CN 112358315A CN 202011361049 A CN202011361049 A CN 202011361049A CN 112358315 A CN112358315 A CN 112358315A
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刘传歆
陈博
李晓强
魏祥庚
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Northwestern Polytechnical University
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    • C04B38/04—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by dissolving-out added substances
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    • 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
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    • 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
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    • 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
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    • C04B2235/5248—Carbon, e.g. graphite

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Abstract

The invention relates to a method for preparing a ceramic matrix composite material containing a cooling pore passage, which comprises the steps of sewing or puncturing a carbon fiber preform by adopting pore-forming fibers capable of being chemically removed to obtain a preset pore-forming fiber composite preform; depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the pore-forming fiber composite preform by adopting a CVI (chemical vapor infiltration) process to obtain a C/SiC composite material; and after polishing to expose the pore-forming fibers, removing the pore-forming fibers by a chemical method to obtain the C/SiC composite material containing the cooling pore channel. The invention adopts the preset pore-forming fiber and the CVI method to prepare the C/SiC composite material containing the cooling pore channel. The method has simple process flow, can prepare complex components, and the C/SiC composite material containing cooling pore channels prepared by the method can adjust process parameters according to specific requirements so as to obtain the C/SiC composite material containing pore channels with required pore channel size and distribution, thereby having great application prospect.

Description

Preparation method of ceramic matrix composite material containing cooling pore channel
Technical Field
The invention belongs to a preparation method of a ceramic matrix composite material, relates to a preparation method of a ceramic matrix composite material containing a cooling duct, and particularly relates to a method for preparing the ceramic matrix composite material containing the cooling duct by utilizing a chemical vapor infiltration process.
Background
The continuous carbon fiber toughened silicon carbide ceramic matrix composite (C/SiC) is a novel strategic heat-proof structure integrated material developed after a carbon/carbon composite (C/C), has the advantages of high temperature resistance, low density, oxidation resistance, high specific strength, specific modulus, corrosion resistance and the like, and becomes a new generation of high-temperature structure candidate material applied to aircraft surface heat protection and hot-end parts of propulsion systems. Taking a scramjet engine as an example, the application of the C/SiC composite material simplifies the structure, reduces the weight, and obviously improves the comprehensive performance of the engine and the effective load of an aircraft, thereby reducing the operation cost of the whole system and being expected to realize the repeated use in a full speed domain. The NASA adopts passive thermal protection measures, and the C/SiC composite material is used for the heat insulation wall of the combustion chamber of the ramjet engine, the front edge of the air inlet and the like, and successfully passes the demonstration and verification of aerospace vehicles such as X-43 and the like. The France SNECMA company adopts the integral nozzle and the nozzle expansion section which are made of C/SiC composite materials, and passes the examination and verification that the inlet temperature of the nozzle is higher than 1800 ℃ and the working time is 900 s. However, passive thermal protection studies have shown that active cooling structures must be developed for longer periods of time or even for repeated use or service at higher mach numbers.
Document 1 "c.bouquet, r.fischer, a.l.bouhali et al.full ceramic composite heat exchange for advanced composite members. aiaa 2005-3433" reports an all-C/SiC composite structure with cooling channels, specifically two C/SiC panels are welded together, a groove is processed on the panel facing the hot gas flow, and two ends of the cold end panel are provided with collecting channels. The structure is flexible, the cross section and the channel of the groove can be adjusted according to requirements so as to meet the requirements of fuel heating and local heat management, and the shape of a component can be made according to the requirements. However, the processing technology is complex, the cost is high, the groove facing the hot gas flow is easy to oxidize, and thermal non-uniformity exists.
Document 2 "m.bouchez, s.beyer.ptah-SOCAR fuel-coated composite Materials structure for dual-mode ramjet and liquid pocket engineering 2005 status. aiaa 2005-. The technology can integrally prepare the combustion chamber, has few connection problems, and is easy to integrate other structural units. However, the heat sink capability of the prepared cooling structure is limited, and the coolant flow needs to be increased aiming at the part with high local heat flow in the flow passage of the scramjet engine, so that the defects of increasing the area of the cooling passage or improving the pressure supply capability of a turbine pump can be caused.
Document 3 "Jihongliang, Zhang Chang Rui, Zhongxin, Cao Ying and preparation and performance of porous C/SiC composite material, novel carbon material 2011, 26(2): 145-150" reports that tungsten filament or glass fiber is used as pore-forming agent, and a pore preset technology is adopted to prepare the sweating porous C/SiC composite material. Due to the fact that the pore presetting technology is adopted, the aperture ratio and the pore structure of the porous C/SiC material can be effectively controlled, and the prepared material has good mechanical property and permeability. However, since the PIP process used in this technique requires a compression molding process, the pre-set pores are bent to some extent, which causes an increase in coolant resistance and a decrease in cooling efficiency.
In addition, patent "ZL 2015108466880.9" reports the channeling of C/SiC composites by ultrashort pulse laser processing techniques. The process has the advantages of small damage to the composite material, high hole forming precision, no recasting layer and the like. However, the ultrashort pulse laser processing technique has low processing efficiency, limited depth of the processed channel and high cost, so that the ultrashort pulse laser processing technique cannot be used commercially in a large scale.
The Chemical Vapor Infiltration (CVI) technology is developed based on Chemical Vapor Deposition (Chemical Vapor Deposition), and means that Chemical reactions occurring on the surface of a porous preform structure during Chemical Vapor Deposition are transferred into the preform structure to generate a ceramic phase in the preform, and the ceramic phase can play a role in filling and bonding. The CVI method has the advantages of low preparation temperature, easy preparation of complex components and the like, and is more and more concerned by people.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a preparation method of a ceramic matrix composite material containing a cooling duct, which realizes the reliable thermal protection of the ceramic matrix composite material under the conditions of high heat flow and low coolant flow, effectively improves the thermal protection capability of a hot end component of a propulsion system and prolongs the service life of the hot end component.
Technical scheme
A preparation method of a ceramic matrix composite material containing a cooling duct is characterized in that the ceramic matrix composite material with a designed cooling duct structure is obtained by presetting the duct, and the steps are as follows:
step 1: sewing or puncturing the carbon fiber preform by adopting pore-forming fibers capable of being chemically removed to obtain a carbon fiber/pore-forming fiber composite preform with a specified shape;
step 2: depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the carbon fiber/pore-forming fiber composite preform by adopting a CVI (chemical vapor infiltration) process to obtain a C/SiC composite material;
the process for preparing the pyrolytic carbon interface phase by the CVI method comprises the following steps: propylene is used as an organic precursor, the total air pressure in the deposition furnace is 1-5 kPa, pyrolytic carbon is deposited within the temperature range of 750-950 ℃, and the deposition time is 10-50 h;
the process for preparing the SiC matrix by the CVI method comprises the following steps: using MTS, i.e. CH3SiCl3As an organic precursor, hydrogen is used as carrier gas and diluent gas, and argon is used as protective gas; the total air pressure in the deposition furnace is 1-5 kPa, SiC is deposited within the temperature range of 900-1200 ℃, and the deposition time is 50-300 h;
and step 3: and (3) polishing the C/SiC composite material to expose pore-forming fibers, and then removing the pore-forming fibers by adopting a chemical method to obtain the C/SiC composite material containing the cooling pore channel.
The chemically removable pore-forming fibers include, but are not limited to, tungsten filaments, molybdenum filaments, or glass filaments.
The diameter of the pore-forming fiber is between 0.05mm and 0.5 mm.
MTS and H of the step 22The molar mixing ratio of (A) to (B) is 1: 5-20。
The chemical process includes, but is not limited to, acid washing.
And the pickling is to remove the tungsten wire by adopting mixed acid pickling of hydrofluoric acid and nitric acid.
And the acid washing is to remove molybdenum wires by adopting aqua regia acid washing.
And the acid cleaning is to remove the glass fiber by adopting hydrofluoric acid.
Advantageous effects
According to the preparation method of the ceramic matrix composite material containing the cooling pore channel, provided by the invention, the pore-forming fiber capable of being chemically removed is adopted to sew or puncture the carbon fiber preform to obtain a preset pore-forming fiber composite preform; depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the pore-forming fiber composite preform by adopting a CVI (chemical vapor infiltration) process to obtain a C/SiC composite material; and after polishing to expose the pore-forming fibers, removing the pore-forming fibers by a chemical method to obtain the C/SiC composite material containing the cooling pore channel.
On the basis of the existing high-temperature resistant passive thermal protection of C/SiC, the controllable sweating cooling runner structure is introduced by giving full play to the characteristic of strong structural design of the composite material, so that the reliable thermal protection under the conditions of high heat flow and low coolant flow is realized, the thermal protection capability of the hot end part of the propulsion system is effectively improved, and the service life of the hot end part is effectively prolonged.
The invention adopts the preset pore-forming fiber and the CVI method to prepare the C/SiC composite material containing the cooling pore channel. The method has simple process flow, can prepare complex components, and the C/SiC composite material containing cooling pore channels prepared by the method can adjust process parameters according to specific requirements so as to obtain the C/SiC composite material containing pore channels with required pore channel size and distribution, thereby having great application prospect.
Drawings
FIG. 1 is a process flow diagram of the process of the present invention
FIG. 2 is a schematic view of the cooling structure of the ceramic matrix composite with channels in the method of the present invention
FIG. 3 is a view of a ceramic matrix composite plate with cooling channels prepared
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example one
Step 1: preparing a carbon fiber preform, and then puncturing or sewing the carbon fiber preform by adopting a tungsten wire (the diameter is 0.1mm) which can be chemically removed to obtain the carbon fiber/tungsten wire composite preform with a specified shape.
Step 2: and (3) depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the carbon fiber/tungsten wire composite preform obtained in the step (1) by adopting a CVI (chemical vapor infiltration) process to obtain the C/SiC composite material. The process for preparing the pyrolytic carbon interface phase by the CVI method comprises the following steps: propylene is used as an organic precursor, the total air pressure in a deposition furnace is 2kPa, pyrolytic carbon is deposited at 800 ℃, and the deposition time is 20 h. The process for preparing the SiC matrix by the CVI method comprises the following steps: using MTS (CH)3SiCl3) As a precursor, hydrogen was used as a carrier gas and a diluent gas, and argon was used as a shielding gas. MTS and H2The molar mixing ratio of (1: 10) and the total gas pressure in the deposition furnace is 5kPa, and the SiC matrix is deposited at 900 ℃ for 100 hours. A
And step 3: and (3) polishing the C/SiC composite material obtained in the step (2) to expose the tungsten wire, and then, pickling by using mixed acid of hydrofluoric acid and nitric acid to remove the tungsten wire, thereby obtaining the C/SiC composite material containing the cooling pore channel.
Example two
Step 1: preparing a carbon fiber preform, and then puncturing or sewing the carbon fiber preform by adopting a tungsten wire (the diameter is 0.2mm) which can be chemically removed to obtain the carbon fiber/tungsten wire composite preform with a specified shape.
Step 2: and (3) depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the carbon fiber/tungsten wire composite preform obtained in the step (1) by adopting a CVI (chemical vapor infiltration) process to obtain the C/SiC composite material. The process for preparing the pyrolytic carbon interface phase by the CVI method comprises the following steps: propylene is used as an organic precursor, the total air pressure in a deposition furnace is 2kPa, pyrolytic carbon is deposited at 850 ℃, and the deposition time is 30 h. The process for preparing the SiC matrix by the CVI method comprises the following steps: using MTS (CH)3SiCl3) As a precursor, hydrogen was used as a carrier gas and a diluent gas, and argon was used as a shielding gas. MTS and H2The molar mixing ratio of (A) to (B) is 1:10, the total gas pressure in the deposition furnace is 5kPa,the SiC matrix was deposited at 1000 ℃ for 150 h.
And step 3: and (3) polishing the C/SiC composite material obtained in the step (2) to expose the tungsten wire, and then, pickling by using mixed acid of hydrofluoric acid and nitric acid to remove the tungsten wire, thereby obtaining the C/SiC composite material containing the cooling pore channel.
EXAMPLE III
Step 1: preparing a carbon fiber preform, and then puncturing or sewing the carbon fiber preform by adopting a tungsten wire (the diameter is 0.5mm) which can be chemically removed to obtain the carbon fiber/tungsten wire composite preform with a specified shape.
Step 2: and (3) depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the carbon fiber/tungsten wire composite preform obtained in the step (1) by adopting a CVI (chemical vapor infiltration) process to obtain the C/SiC composite material. The process for preparing the pyrolytic carbon interface phase by the CVI method comprises the following steps: propylene is used as an organic precursor, the total air pressure in a deposition furnace is 2kPa, pyrolytic carbon is deposited at 900 ℃, and the deposition time is 30 h. The process for preparing the SiC matrix by the CVI method comprises the following steps: using MTS (CH)3SiCl3) As a precursor, hydrogen was used as a carrier gas and a diluent gas, and argon was used as a shielding gas. MTS and H2The molar mixing ratio of (1: 10) and the total gas pressure in the deposition furnace is 5kPa, and the SiC matrix is deposited at 1100 ℃ for 150 hours.
And step 3: and (3) polishing the C/SiC composite material obtained in the step (2) to expose the tungsten wire, and then, pickling by using mixed acid of hydrofluoric acid and nitric acid to remove the tungsten wire, thereby obtaining the C/SiC composite material containing the cooling pore channel.
Example four
Step 1: preparing a carbon fiber preform, and then puncturing or sewing the carbon fiber preform by adopting a molybdenum wire (the diameter is 0.1mm) which can be chemically removed to obtain the carbon fiber/molybdenum wire composite preform with a specified shape.
Step 2: and (3) depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the carbon fiber/molybdenum wire composite preform obtained in the step (1) by adopting a CVI (chemical vapor infiltration) process to obtain the C/SiC composite material. The process for preparing the pyrolytic carbon interface phase by the CVI method comprises the following steps: propylene is used as an organic precursor, the total air pressure in a deposition furnace is 2kPa, pyrolytic carbon is deposited at 800 ℃, and the deposition time is 20 h. CVI processThe process for preparing the SiC matrix comprises the following steps: using MTS (CH)3SiCl3) As a precursor, hydrogen was used as a carrier gas and a diluent gas, and argon was used as a shielding gas. MTS and H2The molar mixing ratio of (1: 10) and the total gas pressure in the deposition furnace is 5kPa, and the SiC matrix is deposited at 900 ℃ for 100 hours.
And step 3: and (3) polishing the C/SiC composite material obtained in the step (2) to expose the molybdenum wire, and then removing the molybdenum wire by adopting aqua regia pickling to obtain the C/SiC composite material containing the cooling pore channel.
EXAMPLE five
Step 1: preparing a carbon fiber preform, and then puncturing or sewing the carbon fiber preform by adopting a molybdenum wire (the diameter is 0.2mm) which can be chemically removed to obtain the carbon fiber/molybdenum wire composite preform with a specified shape.
Step 2: and (3) depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the carbon fiber/molybdenum wire composite preform obtained in the step (1) by adopting a CVI (chemical vapor infiltration) process to obtain the C/SiC composite material. The process for preparing the pyrolytic carbon interface phase by the CVI method comprises the following steps: propylene is used as an organic precursor, the total air pressure in a deposition furnace is 2kPa, pyrolytic carbon is deposited at 900 ℃, and the deposition time is 30 h. The process for preparing the SiC matrix by the CVI method comprises the following steps: using MTS (CH)3SiCl3) As a precursor, hydrogen was used as a carrier gas and a diluent gas, and argon was used as a shielding gas. MTS and H2The molar mixing ratio of (1: 10) and the total gas pressure in the deposition furnace is 5kPa, and the SiC matrix is deposited at 1000 ℃ for 150 hours.
And step 3: and (3) polishing the C/SiC composite material obtained in the step (2) to expose the molybdenum wire, and then removing the molybdenum wire by adopting aqua regia pickling to obtain the C/SiC composite material containing the cooling pore channel.
EXAMPLE six
Step 1: preparing a carbon fiber preform, and then puncturing the carbon fiber preform by adopting chemically removable glass filaments (the diameter is 0.5mm) to obtain the carbon fiber/glass filament composite preform with a specified shape.
Step 2: depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the carbon fiber/glass fiber composite preform obtained in the step 1 by adopting a CVI (chemical vapor infiltration) process to obtain a C/SiC composite preformA material. The process for preparing the pyrolytic carbon interface phase by the CVI method comprises the following steps: propylene is used as an organic precursor, the total air pressure in a deposition furnace is 2kPa, pyrolytic carbon is deposited at 900 ℃, and the deposition time is 30 h. The process for preparing the SiC matrix by the CVI method comprises the following steps: using MTS (CH)3SiCl3) As a precursor, hydrogen was used as a carrier gas and a diluent gas, and argon was used as a shielding gas. MTS and H2The molar mixing ratio of (1: 10) and the total gas pressure in the deposition furnace is 5kPa, and the SiC matrix is deposited at 1100 ℃ for 150 hours.
And step 3: and (3) polishing the C/SiC composite material obtained in the step (2) to expose the glass fiber, and then removing the glass fiber by adopting hydrofluoric acid pickling to obtain the C/SiC composite material containing the cooling pore channel.

Claims (8)

1. A preparation method of a ceramic matrix composite material containing a cooling duct is characterized in that the ceramic matrix composite material with a designed cooling duct structure is obtained by presetting the duct, and the steps are as follows:
step 1: sewing or puncturing the carbon fiber preform by adopting pore-forming fibers capable of being chemically removed to obtain a carbon fiber/pore-forming fiber composite preform with a specified shape;
step 2: depositing and densifying a pyrolytic carbon interface phase and a SiC matrix on the carbon fiber/pore-forming fiber composite preform by adopting a CVI (chemical vapor infiltration) process to obtain a C/SiC composite material;
the process for preparing the pyrolytic carbon interface phase by the CVI method comprises the following steps: propylene is used as an organic precursor, the total air pressure in the deposition furnace is 1-5 kPa, pyrolytic carbon is deposited within the temperature range of 750-950 ℃, and the deposition time is 10-50 h;
the process for preparing the SiC matrix by the CVI method comprises the following steps: using MTS, i.e. CH3SiCl3As an organic precursor, hydrogen is used as carrier gas and diluent gas, and argon is used as protective gas; the total air pressure in the deposition furnace is 1-5 kPa, SiC is deposited within the temperature range of 900-1200 ℃, and the deposition time is 50-300 h;
and step 3: and (3) polishing the C/SiC composite material to expose pore-forming fibers, and then removing the pore-forming fibers by adopting a chemical method to obtain the C/SiC composite material containing the cooling pore channel.
2. The method for preparing a ceramic matrix composite material with cooling channels according to claim 1, wherein: the chemically removable pore-forming fibers include, but are not limited to, tungsten filaments, molybdenum filaments, or glass filaments.
3. The method for preparing a ceramic matrix composite material with cooling channels according to claim 1, wherein: the diameter of the pore-forming fiber is between 0.05mm and 0.5 mm.
4. The method for preparing a ceramic matrix composite material with cooling channels according to claim 1, wherein: MTS and H of the step 22The molar mixing ratio of (A) to (B) is 1: 5-20.
5. The method for preparing a ceramic matrix composite material with cooling channels according to claim 1, wherein: the chemical process includes, but is not limited to, acid washing.
6. The method for preparing a ceramic matrix composite material with cooling channels according to claim 5, wherein: and the pickling is to remove the tungsten wire by adopting mixed acid pickling of hydrofluoric acid and nitric acid.
7. The method for preparing a ceramic matrix composite material with cooling channels according to claim 5, wherein: and the acid washing is to remove molybdenum wires by adopting aqua regia acid washing.
8. The method for preparing a ceramic matrix composite material with cooling channels according to claim 5, wherein: and the acid cleaning is to remove the glass fiber by adopting hydrofluoric acid.
CN202011361049.1A 2020-11-27 2020-11-27 Preparation method of ceramic matrix composite material containing cooling pore channel Pending CN112358315A (en)

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