CN110983208B - C/C-SiC-Cu composite material and preparation method and application thereof - Google Patents

C/C-SiC-Cu composite material and preparation method and application thereof Download PDF

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CN110983208B
CN110983208B CN201911019864.7A CN201911019864A CN110983208B CN 110983208 B CN110983208 B CN 110983208B CN 201911019864 A CN201911019864 A CN 201911019864A CN 110983208 B CN110983208 B CN 110983208B
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CN110983208A (en
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尹健
熊翔
张红波
张欢
徐亚楠
王培�
陈招科
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02—Pretreatment of the fibres or filaments
    • C22C47/06—Pretreatment of the fibres or filaments by forming the fibres or filaments into a preformed structure, e.g. using a temporary binder to form a mat-like element
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/02—Pretreatment of the fibres or filaments
    • C22C47/04—Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/08—Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
    • C22C47/12—Infiltration or casting under mechanical pressure
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments

Abstract

The invention relates to a C/C-SiC-Cu composite material and a preparation method and application thereof. The C/C-SiC-Cu ceramic matrix composite is composed of C fibers, a C matrix, a SiC matrix and a Cu alloy, wherein the C matrix is coated on the C fibers, the SiC matrix is coated on the C matrix, and the Cu alloy is in contact with the SiC matrix to form metallurgical bonding. The preparation method comprises the following steps: the three phases of C, SiC and Cu coexist by combining a chemical vapor infiltration method and a pressure infiltration method. The composite material designed and prepared by the invention has the excellent performances of high strength, high temperature resistance, oxidation resistance, thermal shock resistance, ablation resistance and the like. It is particularly suitable for heat protection components, in particular for heat protection components used on aircraft.

Description

C/C-SiC-Cu composite material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of design and preparation of thermal protective materials, and particularly relates to a C/C-SiC-Cu composite material and a preparation method and application thereof.
Background
The hypersonic speed and sonic speed aircraft is used as a high point in the future aviation field, and the technology of the hypersonic speed and sonic speed aircraft is changed to the world. The novel hypersonic velocity has the characteristics of high reaction speed, strong penetration resistance and high destructiveness. The great military value and the potential commercial value make the method receive wide attention and deep research from the world aerospace strong nation. Sufficiently advanced thermal protection technology enables an aircraft to continue to glide at hypersonic speeds at specific altitudes. Because the flight environment that the aircraft endures in the reentry flight process is severe, and along with the improvement of the performance of the aircraft, higher requirements are also put forward on the thermal protection performance of key parts of the aircraft.
The traditional refractory metal and alloy materials thereof have high density and high thermal conductivity; the C/SiC composite material has the characteristics of low density, high specific strength, ablation resistance and the like, but begins to soften at 2000 ℃; the temperature of the C/C composite material can reach 2800 ℃, but the temperature of the oxidation resistant coating does not exceed 1650 ℃.
The literature' Nenlilna, ablation performance and ablation mechanism of C/C-Cu composite material [ J ]. Chinese non-ferrous metals academic report, 2010,20(3): 510-. The wettability of the molten Cu and the C/C composite material is improved through the active element Ti, and the ablation resistance of the C/C composite material is effectively improved.
The literature "preparation of C/C-SiC composite material and its ablation performance [ J ]. proceedings of shanghai university (nature science edition), 2017,23 (6)" preparation of C/C-SiC composite material by chemical vapor infiltration and precursor impregnation cracking composite process. In the ablation transition region, the molten SiO2 can close the defects of cracks, pores and the like of the material and prevent oxidizing atmosphere from entering the material, so that the material shows excellent ablation resistance. It is required to prepare a novel composite material with ultrahigh temperature resistance, oxidation resistance and ablation resistance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a composite material with excellent mechanical property and ultrahigh temperature resistance as well as a preparation method and application thereof.
The invention relates to a C/C-SiC-Cu ceramic matrix composite, which consists of C fibers, a C matrix, a SiC matrix and a Cu alloy, wherein three phases of C, SiC and Cu coexist in a mode of combining a Chemical Vapor Infiltration (CVI) method and a pressure infiltration method; the C matrix is coated on the C fiber, the SiC matrix is coated on the C matrix, and the Cu alloy composition is in contact with the SiC matrix and forms metallurgical bonding.
According to the C/C-SiC-Cu ceramic matrix composite material, the volume fraction of the C fiber is 15-30%.
According to the C/C-SiC-Cu ceramic matrix composite material, the volume fraction of the C matrix is 10-40%. In the invention, the C matrix is pyrolytic carbon.
According to the C/C-SiC-Cu ceramic matrix composite material, the volume fraction of the SiC matrix is 5% -30%.
According to the C/C-SiC-Cu ceramic matrix composite material, the volume fraction of the Cu matrix is 5-40%.
The invention relates to a preparation method of a C/C-SiC-Cu ceramic matrix composite, which comprises the following steps:
step 1, preparing a carbon fiber preform:
step 1.1, arranging long carbon fiber tows in parallel and uniformly according to a certain direction, weaving certain fiber yarns in the weft direction at certain intervals after gum dipping and gluing treatment, and carrying out edge locking treatment on the edge of the weftless fabric so as to ensure the integrity of the weftless fabric;
step 1.2, selecting chopped carbon fiber bundles with different lengths according to a certain proportion, processing the chopped carbon fiber bundles to form single fibrous filaments, then preparing the fibrous filaments into a fiber net through a net forming process and a net laying process, and prefabricating a net blank;
step 1.3, circularly superposing the non-woven cloth and the net tire obtained in the previous two steps to a certain thickness according to a certain sequence, and then needling the non-woven cloth and the net tire by using a barb pricking pin according to a certain sequence and a pricking depth, so that the fibers in the net tire layer are perpendicularly pricked into the adjacent non-woven cloth layer, and a 2.5D carbon fiber preform is prepared, wherein the density of the preform is 0.30-0.60g/cm 3;
step 2, preparing a C/C porous body: carrying out chemical vapor infiltration deposition on the 2.5D carbon fiber preform obtained in the step 1 for 80-180h to obtain a C/C porous body with the density of 0.6-1.50g/cm3, and then carrying out high-temperature heat treatment under the argon atmosphere, wherein the heat treatment temperature is 2000-2300 ℃;
step 3, preparing a C/C-SiC porous body: placing the C/C porous body obtained in the step (2) in a vapor deposition furnace, wherein the reaction gas is organic silicon, preferably trichloromethylsilane, the deposition temperature is 1200-1300 ℃, and the deposition time is 25-200 h;
step 4, preparing the C/C-SiC-Cu composite material: and (3) obtaining the C/C-SiC-Cu ceramic matrix composite material by adopting a pressure infiltration method for the C/C-SiC ceramic matrix composite material obtained in the step (3), wherein the infiltration temperature is 1100-1300 ℃, and the pressure is 20-40 MPa.
The invention relates to a preparation method of a C/C-SiC-Cu ceramic matrix composite, wherein the flow rates of hydrogen, carrier gas hydrogen and argon introduced in the step 3 are 900-1000 ml/min, preferably 960ml/min, 700-900 ml/min, preferably 720ml/min, 900-1000 ml/min and preferably 960ml/min respectively.
The C/C-SiC-Cu ceramic matrix composite designed and prepared by the invention; the density of the obtained C/C-SiC-Cu ceramic matrix composite material is 2.0 to 2.3g/cm3The thermal conductivity is 4.3-7.2W/M/K, preferably 4.9-7.2W/M/K, and the impact strength is 3, 7-4.4 J.CM-2The compression strength is 102 to 165MPA, preferably 140 to 165MPa, and the bending strength is 97.3 to 199.4 MPa.
The C/C-SiC-Cu ceramic matrix composite designed and prepared by the invention; when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 11.8%, the volume fraction of the SiC matrix is 28%, the volume fraction of the Cu matrix is 8.5% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 6.66 mu g/s and the linear ablation rate is 1 mu m/s; when the ablation time is 20s, the mass ablation speed of the sample is 9.6 mu g/s, and the linear ablation speed is 6.2 mu m/s;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 20%, the volume fraction of the Cu matrix is 8.5% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 8.39 mu g/s and the linear ablation rate is-3.5 mu m/s; when the ablation time is 20s, the mass ablation speed of the sample is 9.27 mu g/s, and the linear ablation speed is-1.8 mu m/s;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 13%, the volume fraction of the Cu matrix is 7.4% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 2.25 mu g/s and the linear ablation rate is-1.6 mu m/s; when the ablation time is 20s, the mass ablation speed of the sample is 1.24 mu g/s, and the linear ablation speed is-0.7 mu m/s;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 9%, the volume fraction of the Cu matrix is 7.8% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 1.8 mu g/s and the linear ablation rate is 1 mu m/s; when the ablation time is 20s, the mass ablation speed of the sample is 11.78 mu g/s, and the linear ablation speed is 8 mu m/s;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 5%, the volume fraction of the Cu matrix is 8.5% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 8.64 mu g/s and the linear ablation rate is 8.3 mu m/s; when the ablation time is 20s, the mass ablation rate of the sample is 12.65 mug/s, and the linear ablation rate is 11.6 mug/s.
The invention relates to a C/C-SiC-Cu ceramicIn the preparation method of the matrix composite material, in the C/C-SiC-Cu ceramic matrix composite material, the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 11.8%, the volume fraction of the SiC matrix is 28%, the volume fraction of the Cu matrix is 8.5%, the thermal conductivity of the matrix composite material is 4.89W/M/K, and the impact strength of the matrix composite material is 4.4 J.CM-2The compressive strength is 145.8MPa, and the bending strength is 166.5 MPa;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 20%, the volume fraction of the Cu matrix is 8.5% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the thermal conductivity is 7.156W/M/K and the impact strength is 4.133 J.CM-2The compression strength is 164.8MPa, and the bending strength is 199.4 MPa;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 13%, the volume fraction of the Cu matrix is 7.4% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the thermal conductivity is 6.8W/M/K and the impact strength is 3.7 J.CM-2The compression strength is 147.5MPa, and the bending strength is 131.4 MPa;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 9%, the volume fraction of the Cu matrix is 7.8% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the thermal conductivity is 5.23W/M/K and the impact strength is 3.9 J.CM-2The compression strength is 122.1MPa, and the bending strength is 124.1 MPa;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 5%, the volume fraction of the Cu matrix is 8.5% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the thermal conductivity is 4.325W/M/K and the impact strength is 4.2 J.CM-2The compressive strength was 105MPa, and the bending strength was 97.4 MPa.
The C/C-SiC-Cu ceramic matrix composite designed and prepared by the invention; it can be used for heat shielding components. Preferably, the heat protection component is a heat protection component used on an aircraft.
Principles and advantages
The invention controls the volume fraction of the C fiber to be 15-30%, the volume fraction of the C matrix to be 10-40%, the volume fraction of the SiC matrix to be 5-30% and the volume fraction of the Cu matrix to be 5-40%; the product with excellent performance is obtained by combining the preparation process and reasonable condition parameters.
After optimization, when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 13%, the volume fraction of the Cu matrix is 7.4% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 2.25 mu g/s and the linear ablation rate is-1.6 mu m/s; when the composite material is ablated for 20s, the mass ablation rate of the sample is 1.24 mu g/s, the linear ablation rate is-0.7 mu m/s, and when the volume fraction of the C fibers in the C/C-SiC-Cu ceramic matrix composite material is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 20%, the volume fraction of the Cu matrix is 8.5%, and the balance is uniformly distributed pores, the ablation rate is detected according to the national standard GJB323A-96 at 2500 ℃, and when the composite material is ablated for 10s, the mass ablation rate of the sample is 8.39 mu g/s, and the linear ablation rate is-3.5 mu m/s; when the ablation time is 20s, the mass ablation rate of the sample is 9.27 mu g/s, and the linear ablation rate is-1.8 mu m/s. This is well beyond the experimental expectations at the time. In particular, the composite material is not a fully dense material, but the composite material is processed according to the national standard GJB323A-96, and the mass ablation speed of the composite material in 20s ablation is found to be far lower than that in 10s ablation in the detection process, which is completely beyond the expectation.
Drawings
FIG. 1 is a flow chart of the preparation of the C/C-SiC-Cu composite material designed by the present invention;
FIG. 2 is a microstructure topography of the sample obtained in example 1.
FIG. 3 is a microstructure topography of the sample obtained in example 2.
Detailed Description
The present invention will be described in detail with reference to the following examples and accompanying drawings.
Example 1
A C/C-SiC-Cu composite material consists of C fibers, a C matrix, a SiC matrix and a Cu alloy, and is characterized in that three phases of C, SiC and Cu coexist by combining a Chemical Vapor Infiltration (CVI) method and a pressure infiltration method. The volume fraction of the C fiber is 26%, the volume fraction of the C matrix is 11.8%, the volume fraction of the SiC matrix is 28%, the volume fraction of the Cu matrix is 8.5%, and the balance is uniformly distributed pores.
In this embodiment, the preparation of the designed C/C-SiC-Cu composite material includes the following sequential steps:
step 1, preparing a carbon fiber preform:
step 1.1, arranging long carbon fiber tows in parallel and uniformly according to a certain direction, weaving certain fiber yarns in the weft direction at certain intervals after gum dipping and gluing treatment, and carrying out edge locking treatment on the edge of the weftless fabric so as to ensure the integrity of the weftless fabric;
step 1.2, selecting chopped carbon fiber bundles with different lengths according to a certain proportion, processing the chopped carbon fiber bundles to form single fibrous filaments, then preparing the fibrous filaments into a fiber net through a net forming process and a net laying process, and prefabricating a net blank;
step 1.3, circularly superposing the non-woven fabric and the mesh tire obtained in the previous two steps to a certain thickness according to a certain sequence, and then needling the non-woven fabric and the mesh tire by using a barb and felting needle according to a certain sequence and penetration depth to ensure that fibers in the mesh tire layer are vertically penetrated into the adjacent non-woven fabric layer, so that a 2.5D carbon fiber preform is prepared, wherein the density of the preform is 0.45g/cm 3;
step 2, preparing a C/C porous body: pyrolyzing carbon for 150 hours by chemical vapor infiltration deposition on the carbon fiber preform obtained in the step 1 to obtain a C/C porous body with the density of 0.68g/cm3, and then carrying out high-temperature heat treatment in an argon atmosphere, wherein the heat treatment temperature is 2000-2300 ℃;
step 3, preparing the C/C-SiC ceramic matrix composite material: placing the C/C porous body obtained in the step 2 in a vapor deposition furnace, wherein the reaction gas is trichloromethylsilane, the deposition temperature is 1250 ℃, and the deposition time is 150 h;
step 4, preparing the C/C-SiC-Cu ceramic matrix composite material: and 3, obtaining the C/C-SiC-Cu ceramic matrix composite material by adopting a pressure infiltration method for the C/C-SiC ceramic matrix composite material obtained in the step 3, wherein the infiltration temperature is 1150 ℃, and the pressure is 20 MPa.
The flow rates of introducing hydrogen for dilution, hydrogen for carrier gas and argon for preparing the C/C-SiC composite material are 960ml/min, 720ml/min and 960ml/min respectively.
The microstructure of the obtained C/C-SiC-Cu ceramic matrix composite is shown in figure 2, the interface combination of the carbon fiber and pyrolytic carbon, the interface combination of the pyrolytic carbon and SiC, and the interface combination of SiC and a copper alloy matrix is good, no obvious defect is found, and the compactness of the composite is good. The density was 2.27g/cm3The thermal conductivity is 4.89W/M/K, and the impact strength is 4.4 J.CM-2The compressive strength was 145.8MPa and the bending strength was 166.5 MPa. Detecting the ablation rate (according to the national standard GJB 323A-96) at 2500 ℃, wherein when the ablation is carried out for 10s, the mass ablation speed of the sample is 6.66 mu g/s, and the linear ablation speed is 1 mu m/s; when the ablation time is 20s, the mass ablation rate of the sample is 9.6 mu g/s, and the linear ablation rate is 6.2 mu m/s.
Example 2
A C/C-SiC-Cu composite material consists of C fibers, a C matrix, a SiC matrix and a Cu alloy, and is characterized in that three phases of C, SiC and Cu coexist by combining a Chemical Vapor Infiltration (CVI) method and a pressure infiltration method. The volume fraction of the C fiber is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 20%, and the volume fraction of the Cu matrix is 8.5%.
In this embodiment, the preparation of the designed C/C-SiC-Cu composite material includes the following sequential steps:
step 1, preparing a carbon fiber preform:
step 1.1, arranging long carbon fiber tows in parallel and uniformly according to a certain direction, after gum dipping and gluing, weaving certain fiber yarns in the weft direction at certain intervals, and performing overlocking treatment on the edges of the non-woven fabric to ensure the integrity of the non-woven fabric;
step 1.2, selecting chopped carbon fiber bundles with different lengths according to a certain proportion, processing the chopped carbon fiber bundles to form single fibrous filaments, then preparing the fibrous filaments into a fiber net through a net forming process and a net laying process, and prefabricating a net blank;
step 1.3, circularly superposing the non-woven fabric and the net tire obtained in the previous two steps to a certain thickness according to a certain sequence, and then needling the non-woven fabric and the net tire by using a barb and felting needle according to a certain sequence and penetration depth to ensure that fibers in a net tire layer are vertically penetrated into an adjacent non-woven fabric layer, so that a 2.5-dimensional carbon fiber preform is prepared, wherein the density of the preform is 0.45g/cm 3;
step 2, preparing a C/C porous body: pyrolyzing carbon for 180 hours by chemical vapor infiltration deposition of the carbon fiber preform obtained in the step 1 to obtain a C/C porous body with the density of 0.98g/cm3, and then carrying out high-temperature heat treatment in an argon atmosphere, wherein the heat treatment temperature is 2000-2300 ℃;
step 3, preparing the C/C-SiC ceramic matrix composite material: placing the C/C porous body obtained in the step 2 in a vapor deposition furnace, wherein the reaction gas is trichloromethylsilane, the deposition temperature is 1250 ℃, and the deposition time is 150 h;
step 4, preparing the C/C-SiC-Cu ceramic matrix composite material: and 3, obtaining the C/C-SiC-Cu ceramic matrix composite material by adopting a pressure infiltration method for the C/C-SiC ceramic matrix composite material obtained in the step 3, wherein the infiltration temperature is 1150 ℃, and the pressure is 20 MPa.
The flow rates of introducing hydrogen for dilution, hydrogen for carrier gas and argon for preparing the C/C-SiC composite material are 960ml/min, 720ml/min and 960ml/min respectively.
The microstructure of the obtained C/C-SiC-Cu ceramic matrix composite is shown in figure 3, the interface combination of the carbon fiber and pyrolytic carbon, the interface combination of the pyrolytic carbon and SiC, and the interface combination of SiC and a copper alloy matrix is good, no obvious defect is found, and the compactness of the composite is good. The density was 23g/cm3The thermal conductivity is 7.156W/M/K, and the impact strength is 4.133 J.CM-2The compressive strength was 164.8MPa, and the bending strength was 199.4 MPa. Ablation rate was measured at 2500 ℃ (according to the national standard GJB323A-96), when the ablation is carried out for 10s, the mass ablation speed of the sample is 8.39 mu g/s, and the linear ablation speed is-3.5 mu m/s; when the ablation time is 20s, the mass ablation rate of the sample is 9.27 mu g/s, and the linear ablation rate is-1.8 mu m/s.
Example 3
A C/C-SiC-Cu composite material consists of C fibers, a C matrix, a SiC matrix and a Cu alloy, and is characterized in that three phases of C, SiC and Cu coexist by combining a Chemical Vapor Infiltration (CVI) method and a pressure infiltration method. The volume fraction of the C fiber is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 13%, and the volume fraction of the Cu matrix is 7.4%.
In this embodiment, the preparation of the designed C/C-SiC-Cu composite material includes the following sequential steps:
step 1, preparing a carbon fiber preform:
step 1.1, arranging long carbon fiber tows in parallel and uniformly according to a certain direction, after gum dipping and gluing, weaving certain fiber yarns in the weft direction at certain intervals, and performing overlocking treatment on the edges of the non-woven fabric to ensure the integrity of the non-woven fabric;
step 1.2, selecting chopped carbon fiber bundles with different lengths according to a certain proportion, processing the chopped carbon fiber bundles to form single fibrous filaments, then preparing the fibrous filaments into a fiber net through a net forming process and a net laying process, and prefabricating a net blank;
step 1.3, circularly superposing the non-woven fabric and the net tire obtained in the previous two steps to a certain thickness according to a certain sequence, and then needling the non-woven fabric and the net tire by using a barb and felting needle according to a certain sequence and penetration depth to ensure that fibers in a net tire layer are vertically penetrated into an adjacent non-woven fabric layer, so that a 2.5-dimensional carbon fiber preform is prepared, wherein the density of the preform is 0.45g/cm 3;
step 2, preparing a C/C porous body: pyrolyzing carbon for 180 hours by chemical vapor infiltration deposition of the carbon fiber preform obtained in the step 1 to obtain a C/C porous body with the density of 0.98g/cm3, and then carrying out high-temperature heat treatment in an argon atmosphere, wherein the heat treatment temperature is 2000-2300 ℃;
step 3, preparing the C/C-SiC ceramic matrix composite material: placing the C/C porous body obtained in the step 2 in a vapor deposition furnace, wherein the reaction gas is trichloromethylsilane, the deposition temperature is 1250 ℃, and the deposition time is 100 hours;
step 4, preparing the C/C-SiC-Cu ceramic matrix composite material: and 3, obtaining the C/C-SiC-Cu ceramic matrix composite material by adopting a pressure infiltration method for the C/C-SiC ceramic matrix composite material obtained in the step 3, wherein the infiltration temperature is 1150 ℃, and the pressure is 20 MPa.
The flow rates of introducing hydrogen for dilution, hydrogen for carrier gas and argon for preparing the C/C-SiC composite material are 960ml/min, 720ml/min and 960ml/min respectively.
The obtained C/C-SiC-Cu ceramic matrix composite has good interface bonding of carbon fiber and pyrolytic carbon, pyrolytic carbon and SiC, and SiC and copper alloy matrix, no obvious defect is found, and the composite has good compactness. The density was 2.18g/cm3The thermal conductivity is 6.8W/M/K, and the impact strength is 3.7 J.CM-2The compressive strength was 147.5MPa, and the bending strength was 131.4 MPa. Detecting the ablation rate (according to the national standard GJB 323A-96) at 2500 ℃, wherein the mass ablation rate of the sample is 2.25 mu g/s and the linear ablation rate is-1.6 mu m/s when the sample is ablated for 10 s; when the ablation time is 20s, the mass ablation rate of the sample is 1.24 mu g/s, and the linear ablation rate is-0.7 mu m/s.
Example 4
A C/C-SiC-Cu composite material consists of C fibers, a C matrix, a SiC matrix and a Cu alloy, and is characterized in that three phases of C, SiC and Cu coexist by combining a Chemical Vapor Infiltration (CVI) method and a pressure infiltration method. The volume fraction of the C fiber is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 9%, and the volume fraction of the Cu matrix is 7.8%.
In this embodiment, the preparation of the designed C/C-SiC-Cu composite material includes the following sequential steps:
step 1, preparing a carbon fiber preform:
step 1.1, arranging long carbon fiber tows in parallel and uniformly according to a certain direction, after gum dipping and gluing, weaving certain fiber yarns in the weft direction at certain intervals, and performing overlocking treatment on the edges of the non-woven fabric to ensure the integrity of the non-woven fabric;
step 1.2, selecting chopped carbon fiber bundles with different lengths according to a certain proportion, processing the chopped carbon fiber bundles to form single fibrous filaments, then preparing the fibrous filaments into a fiber net through a net forming process and a net laying process, and prefabricating a net blank;
step 1.3, circularly superposing the non-woven fabric and the net tire obtained in the previous two steps to a certain thickness according to a certain sequence, and then needling the non-woven fabric and the net tire by using a barb and felting needle according to a certain sequence and penetration depth to ensure that fibers in a net tire layer are vertically penetrated into an adjacent non-woven fabric layer, so that a 2.5-dimensional carbon fiber preform is prepared, wherein the density of the preform is 0.45g/cm 3;
step 2, preparing a C/C porous body: pyrolyzing carbon for 180 hours by chemical vapor infiltration deposition of the carbon fiber preform obtained in the step 1 to obtain a C/C porous body with the density of 0.98g/cm3, and then carrying out high-temperature heat treatment in an argon atmosphere, wherein the heat treatment temperature is 2000-2300 ℃;
step 3, preparing the C/C-SiC ceramic matrix composite material: placing the C/C porous body obtained in the step 2 in a vapor deposition furnace, wherein the reaction gas is trichloromethylsilane, the deposition temperature is 1250 ℃, and the deposition time is 50 h;
step 4, preparing the C/C-SiC-Cu ceramic matrix composite material: and 3, obtaining the C/C-SiC-Cu ceramic matrix composite material by adopting a pressure infiltration method for the C/C-SiC ceramic matrix composite material obtained in the step 3, wherein the infiltration temperature is 1150 ℃, and the pressure is 20 MPa.
The flow rates of introducing hydrogen for dilution, hydrogen for carrier gas and argon for preparing the C/C-SiC composite material are 960ml/min, 720ml/min and 960ml/min respectively.
The obtained C/C-SiC-Cu ceramic matrix composite has good interface bonding of carbon fiber and pyrolytic carbon, pyrolytic carbon and SiC, and SiC and copper alloy matrix, no obvious defect is found, and the composite has good compactness. The density was 2.01g/cm3The thermal conductivity is 5.23W/M/K, and the impact strength is 3.9 J.CM-2The compressive strength was 122.1MPa and the bending strength was 124.1 MPa. Detecting the ablation rate (according to the national standard GJB 323A-96) at 2500 ℃, wherein when the ablation is carried out for 10s, the mass ablation speed of the sample is 1.8 mu g/s, and the linear ablation speed is 1 mu m/s; when ablating for 20sThe mass ablation rate of the sample was 11.78. mu.g/s, and the linear ablation rate was 8 μm/s.
Example 5
A C/C-SiC-Cu composite material consists of C fibers, a C matrix, a SiC matrix and a Cu alloy, and is characterized in that three phases of C, SiC and Cu coexist by combining a Chemical Vapor Infiltration (CVI) method and a pressure infiltration method. The volume fraction of the C fiber is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 5%, and the volume fraction of the Cu matrix is 8.5%.
In this embodiment, the preparation of the designed C/C-SiC-Cu composite material includes the following sequential steps:
step 1, preparing a carbon fiber preform:
step 1.1, arranging long carbon fiber tows in parallel and uniformly according to a certain direction, after gum dipping and gluing, weaving certain fiber yarns in the weft direction at certain intervals, and performing overlocking treatment on the edges of the non-woven fabric to ensure the integrity of the non-woven fabric;
step 1.2, selecting chopped carbon fiber bundles with different lengths according to a certain proportion, processing the chopped carbon fiber bundles to form single fibrous filaments, then preparing the fibrous filaments into a fiber net through a net forming process and a net laying process, and prefabricating a net blank;
step 1.3, circularly superposing the non-woven fabric and the net tire obtained in the previous two steps to a certain thickness according to a certain sequence, and then needling the non-woven fabric and the net tire by using a barb and felting needle according to a certain sequence and penetration depth to ensure that fibers in a net tire layer are vertically penetrated into an adjacent non-woven fabric layer, so that a 2.5-dimensional carbon fiber preform is prepared, wherein the density of the preform is 0.45g/cm 3;
step 2, preparing a C/C porous body: pyrolyzing carbon for 180 hours by chemical vapor infiltration deposition of the carbon fiber preform obtained in the step 1 to obtain a C/C porous body with the density of 0.98g/cm3, and then carrying out high-temperature heat treatment in an argon atmosphere, wherein the heat treatment temperature is 2000-2300 ℃;
step 3, preparing the C/C-SiC ceramic matrix composite material: placing the C/C porous body obtained in the step 2 in a vapor deposition furnace, wherein the reaction gas is trichloromethylsilane, the deposition temperature is 1250 ℃, and the deposition time is 25 hours;
step 4, preparing the C/C-SiC-Cu ceramic matrix composite material: and 3, obtaining the C/C-SiC-Cu ceramic matrix composite material by adopting a pressure infiltration method for the C/C-SiC ceramic matrix composite material obtained in the step 3, wherein the infiltration temperature is 1150 ℃, and the pressure is 20 MPa.
The flow rates of introducing hydrogen for dilution, hydrogen for carrier gas and argon for preparing the C/C-SiC composite material are 960ml/min, 720ml/min and 960ml/min respectively.
The obtained C/C-SiC-Cu ceramic matrix composite has good interface bonding of carbon fiber and pyrolytic carbon, pyrolytic carbon and SiC, and SiC and copper alloy matrix, no obvious defect is found, and the composite has good compactness. The density was 1.94g/cm3The thermal conductivity is 4.325W/M/K, and the impact strength is 4.2 J.CM-2The compressive strength was 105MPa, and the bending strength was 97.4 MPa. Detecting the ablation rate (according to the national standard GJB 323A-96) at 2500 ℃, wherein when the ablation is carried out for 10s, the mass ablation speed of the sample is 8.64 mu g/s, and the linear ablation speed is 8.3 mu m/s; when the ablation time is 20s, the mass ablation rate of the sample is 12.65 mug/s, and the linear ablation rate is 11.6 mug/s.

Claims (8)

1. A C/C-SiC-Cu ceramic matrix composite material is characterized in that: the C/C-SiC-Cu ceramic matrix composite consists of C fibers, a C matrix, a SiC matrix and a Cu alloy, and three phases of C, SiC and Cu coexist in a mode of combining a chemical vapor infiltration method and a pressure infiltration method; the C matrix is coated on the C fiber, the SiC matrix is coated on the C matrix, and the Cu alloy is in contact with the SiC matrix to form metallurgical bonding;
the volume fraction of the C fiber is 15-30%;
the volume fraction of the C matrix is 10-40%;
the SiC matrix accounts for 5 to 30 percent of the volume fraction;
the volume fraction of the Cu alloy is 5-40%;
the C/C-SiC-Cu ceramic matrix composite is prepared by the following steps:
step 1, preparing a carbon fiber preform:
step 1.1, arranging long carbon fiber tows in parallel and uniformly according to a certain direction, weaving certain fiber yarns in the weft direction at certain intervals after gum dipping and gluing treatment, and carrying out edge locking treatment on the edge of the weftless fabric so as to ensure the integrity of the weftless fabric;
step 1.2, selecting chopped carbon fiber bundles with different lengths according to a certain proportion, processing the chopped carbon fiber bundles to form single fibrous filaments, then preparing the fibrous filaments into a fiber net through a net forming process and a net laying process, and prefabricating a net blank;
step 1.3, circularly superposing the non-woven cloth and the net tire obtained in the previous two steps to a certain thickness according to a certain sequence, and then needling the non-woven cloth and the net tire by using the barb pricking pins according to a certain sequence and a certain pricking depth to ensure that the fibers in the net tire layer are perpendicularly pricked into the adjacent non-woven cloth layer, thereby preparing a 2.5D carbon fiber preform with the density of 0.30-0.60g/cm3；
Step 2, preparing a C/C porous body: pyrolyzing carbon by chemical vapor infiltration deposition on the 2.5D carbon fiber preform obtained in the step 1 to obtain the carbon fiber preform with the density of 0.7-1.50 g/cm3The C/C porous body is subjected to high-temperature heat treatment in an argon atmosphere, wherein the heat treatment temperature is 2000-2300 ℃;
step 3, preparing a C/C-SiC porous body: placing the C/C porous body obtained in the step 2 in a vapor deposition furnace, wherein the reaction gas is organic silicon, the deposition temperature is 1200-1300 ℃, and the deposition time is 25-200 h;
step 4, preparing the C/C-SiC-Cu composite material: and (3) obtaining the C/C-SiC-Cu ceramic matrix composite material by adopting a pressure infiltration method for the C/C-SiC ceramic matrix composite material obtained in the step (3), wherein the infiltration temperature is 1100-1300 ℃, and the pressure is 20-40 MPa.
2. The C/C-SiC-Cu ceramic matrix composite according to claim 1, characterized in that: the C/C-SiC-Cu ceramic matrix composite contains uniformly distributed pores, and the porosity of the C/C-SiC-Cu ceramic matrix composite is 20% -35%.
3. The C/C-SiC-Cu ceramic matrix composite according to claim 2, characterized in that: the C/C-SiC-Cu ceramic matrix composite contains uniformly distributed pores, and the porosity of the C/C-SiC-Cu ceramic matrix composite is 20% -21%.
4. The C/C-SiC-Cu ceramic matrix composite according to claim 1, characterized in that: and 3, introducing hydrogen for dilution, hydrogen for carrier gas and argon respectively at the flow rates of 900-1000 mL/min, 700-900 mL/min and 900-1000 mL/min.
5. The C/C-SiC-Cu ceramic matrix composite according to claim 1, characterized in that: the density of the obtained C/C-SiC-Cu ceramic matrix composite material is 2.0 to 2.3g/cm3The thermal conductivity is 4.3 to 7.2W/m/K, and the impact strength is 3.7 to 4.4J-cm-2The compression strength is 102-165 MPa, and the bending strength is 97.3-199.4 MPa.
6. The C/C-SiC-Cu ceramic matrix composite according to claim 1, characterized in that: when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 11.8%, the volume fraction of the SiC matrix is 28%, the volume fraction of the Cu alloy is 8.5% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite material, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 6.66 mu g/s and the linear ablation rate is 1 mu m/s; when the ablation time is 20s, the mass ablation speed of the sample is 9.6 mu g/s, and the linear ablation speed is 6.2 mu m/s;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 20%, the volume fraction of the Cu alloy is 8.5% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite material, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 8.39 mu g/s and the linear ablation rate is-3.5 mu m/s; when the ablation time is 20s, the mass ablation speed of the sample is 9.27 mu g/s, and the linear ablation speed is-1.8 mu m/s;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 13%, the volume fraction of the Cu alloy is 7.4% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite material, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 2.25 mu g/s and the linear ablation rate is-1.6 mu m/s; when the ablation time is 20s, the mass ablation speed of the sample is 1.24 mu g/s, and the linear ablation speed is-0.7 mu m/s;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 9%, the volume fraction of the Cu alloy is 7.8% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite material, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 1.8 mu g/s and the linear ablation rate is 1 mu m/s; when the ablation time is 20s, the mass ablation speed of the sample is 11.78 mu g/s, and the linear ablation speed is 8 mu m/s;
when the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 5%, the volume fraction of the Cu alloy is 8.5% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite material, the ablation rate is detected at 2500 ℃ according to the national standard GJB323A-96, and when the ablation lasts for 10s, the mass ablation rate of a sample is 8.64 mu g/s and the linear ablation rate is 8.3 mu m/s; when the ablation time is 20s, the mass ablation rate of the sample is 12.65 mug/s, and the linear ablation rate is 11.6 mug/s.
7. The C/C-SiC-Cu ceramic matrix composite according to claim 1, characterized in that: when the C/C-SiC-Cu ceramic matrix composite material is prepared, the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 11.8%, the volume fraction of the SiC matrix is 28%, the volume fraction of the Cu alloy is 8.5%, the thermal conductivity of the Cu alloy is 4.89W/m/K, and the impact strength of the Cu alloy is 4.4J-cm-2The compressive strength is 145.8MPa, and the bending strength is 166.5 MPa;
when the C/C-SiC-Cu ceramic matrix composite material is prepared, the volume fraction of the C fibers is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 20%, and C isThe volume fraction of the u alloy is 8.5%, and the rest is uniformly distributed pores, the thermal conductivity is 7.156W/m/K, and the impact strength is 4.133J cm-2The compression strength is 164.8MPa, and the bending strength is 199.4 MPa;
when the volume fraction of the C fiber is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 13%, the volume fraction of the Cu alloy is 7.4% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite material, the thermal conductivity is 6.8W/m/K and the impact strength is 3.7J-cm-2The compression strength is 147.5MPa, and the bending strength is 131.4 MPa;
when the volume fraction of the C fiber is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 9%, the volume fraction of the Cu alloy is 7.8% and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite material, the thermal conductivity is 5.23W/m/K, and the impact strength is 3.9J-cm-2The compression strength is 122.1MPa, and the bending strength is 124.1 MPa;
when the volume fraction of the C fiber is 26%, the volume fraction of the C matrix is 27.1%, the volume fraction of the SiC matrix is 5%, the volume fraction of the Cu alloy is 8.5%, and the balance is uniformly distributed pores in the C/C-SiC-Cu ceramic matrix composite, the thermal conductivity is 4.325W/m/K, and the impact strength is 4.2J-cm-2The compressive strength was 105MPa, and the bending strength was 97.4 MPa.
8. Use of a C/C-SiC-Cu ceramic matrix composite material according to any one of claims 1 to 4, characterized in that: the C/C-SiC-Cu ceramic matrix composite material is used for a thermal protection component.
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