CN115417699A - Preparation method of PyC-SiC-HfC three-interface-phase modified C/C-SiBCN double-matrix ablation-resistant composite material - Google Patents
Preparation method of PyC-SiC-HfC three-interface-phase modified C/C-SiBCN double-matrix ablation-resistant composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a PyC-SiC-HfC three-interface phase modified C/C-SiBCN double-matrix ablation-resistant composite material, which comprises PyC-SiC-HfC interface phase preparation and C-SiBCN matrix preparation, and specifically comprises the following steps: (1) Preparing a PyC + SiC interface phase on the fiber surface of the carbon fiber preform by using a CVD (chemical vapor deposition) process to obtain a preform with an interface phase with a certain thickness; (2) Dipping the prefabricated body prepared in the step (1) in an HfC polymer-xylene solution for multiple times to prepare a PyC-SiC-HfC three-interface phase modified carbon fiber prefabricated body material; (3) preparing a C matrix by a CVI process; (4) preparing a SiBCN modified matrix through a PIP process; (5) curing and cracking; (6) And (5) repeating the steps (4) and (5) to finally obtain the C/PyC-SiC-HfC/C-SiBCN composite material. The invention adopts a three-interface phase complementary high-temperature resistant system of PyC-SiC-HfC, and utilizes the good lamellar structure of PyC, the good ablation resistance of HfC and the good thermal expansion coefficient matching capability of SiC as the interface phase of the C/C-SiBCN composite material, thereby improving the ablation resistance of the whole composite material.
Description
Technical Field
The invention discloses a preparation method of a PyC-SiC-HfC three-interface phase modified C/C-SiBCN double-matrix ablation-resistant composite material.
Background
The hypersonic aircraft is the main development direction of aerospace, and as the aircraft moves for a long time at a high speed in the atmosphere, the generated high-mach pneumatic heating and high-temperature air flow heating put high requirements on structural materials of the aircraft, and the protective material is required to have good performances of light weight, high strength and excellent ablation resistance.
The C fiber reinforced C matrix composite material is a commonly-known C/C composite material, and is a composite material which is prepared by processing carbon fibers or carbon fiber fabrics such as carbon cloth, carbon felt and the like serving as a reinforcement and C serving as a matrix through a Chemical Vapor Infiltration (CVI) process and has the advantages of low density, high specific strength, high modulus, high heat conductivity, high specific heat capacity, excellent thermal shock resistance, excellent wear resistance and the like. Due to the low oxidation temperature of the carbon material, the commonly used method for improving the ablation resistance of the C/C composite material mainly aims at improving the carbon fiber preform and pyrolytic carbon texture technology, the matrix modification technology and the external ablation-resistant coating counting, and the method for modifying the multi-interface phase and combining the matrix phase is rarely researched.
Two composite material protection systems are divided according to the protection mechanism of the ablation-resistant composite material: coating material systems and fiber/matrix modification systems. For a coating material system, the coating material itself needs to have the characteristics of higher melting point, higher mechanical property, better adhesiveness, proper expansion coefficient and the like, and according to the characteristics, the coating materials commonly used at present can be divided into the following categories according to the main components, wherein the categories are as follows: silicon-based ceramic coatings, boron-based ceramic coatings, metal oxide coatings, metal carbide coatings, and the like.
The fiber/matrix modification system of the C/C composite material can be further divided into matrix phase modification and interface phase modification: the matrix is modified by introducing SiC, hfC, zrC and ZrB into the matrix 2 、MoSi 2 Or one or more of other metal ions, can be divided into single-phase, two-phase, multi-phase and metal element modified C/C composite materials, and the matrix modification system of the C/C composite material has the advantages compared with the interface phase: the requirement for strong bonding force of the interface phase and the matrix material is reduced, and although the doping material and the matrix material are still required to have similar thermal expansion coefficients, the strict requirement on the expansion coefficient is reduced because the dopants are more dispersed.
The interface phase modification process is an ablation-resistant material modification process proposed based on the starting point of fiber protection, and the ablation resistance of the composite material is generally influenced by the matrix, the fibers and the interface between the matrix and the fibers. The interface tends to have larger specific surface area and higher interface energy, so the interface tends to become a weak phase in the C/C composite material, and after the fiber is ablated into a needle point shape, the whole ablation surface tends to form an integral receding form. Generally, the graphitized carbon layer structure is suitable for use as an interface phase of a C/C composite, which provides a weaker chemical bond between the carbon fiber and the carbon matrix, necessary to promote toughening. In order to protect the carbon fibers, a BN or SiC interface with a certain thickness is often prepared at the fiber interface, and oxidation products of the two interfaces are utilized to protect the fibers, so that the ablation resistance of the composite material is further enhanced.
Disclosure of Invention
The invention aims to provide a preparation method of a PyC-SiC-HfC three-interface phase modified C/C-SiBCN double-matrix ablation-resistant composite material, which solves the problems in the prior art.
The invention can be solved by the following technical scheme:
a preparation method of a PyC-SiC-HfC three-interface phase modified C/C-SiBCN double-matrix ablation-resistant composite material comprises PyC-SiC-HfC interface phase preparation and C-SiBCN matrix preparation, and specifically comprises the following steps: (1) Preparing a PyC + SiC interface phase on the fiber surface of the carbon fiber preform by using a CVD (chemical vapor deposition) process to obtain a preform with an interface phase with a certain thickness; (2) Dipping the prefabricated body prepared in the step (1) in an HfC polymer-xylene solution for multiple times to prepare a PyC-SiC-HfC three-interface phase modified carbon fiber prefabricated body material; (3) preparing a C matrix by a CVI process; (4) preparing a SiBCN modified matrix through a PIP process; (5) curing and cracking; (6) And (5) repeating the steps (4) and (5) to finally obtain the C/PyC-SiC-HfC/C-SiBCN composite material.
Further, the carbon fiber preform is a 2D laminated carbon fiber.
Further, the carbon source selected for deposition of PyC interface is C 3 H 6 Or CH 4 The deposition pressure of alkane gas is 10-20KPa, the deposition time is 10-15h, the deposition temperature is 950-1000 ℃, and the deposition residence time is 0.5-1s.
Further, the gas source selected for depositing the SiC interface is MTS + H 2 +N 2 The deposition pressure is 10-20KPa, the temperature is 1050 ℃, and the deposition time is 12-15h.
Further, in the step 2), the time for soaking in the HfC polymer-xylene solution is 2-5h, the soaking mass fraction is 13-15, and the heat treatment temperature is 1500-1600 ℃ according to the temperature for generating the hafnium carbide crystal.
Further, in the step 3), the designed density of the carbon matrix is 1.2-1.4g/cm 3 The selected gas source is CH 4 Or C 3 H 6 The deposition pressure of the alkane gas is 100-200mbar, the gas retention time is 0.5-1s, and the deposition time is 10-14h.
Further, in the step 4), the boron content of the polyborosilazane precursor is between 1 and 2 percent, the viscosity is within the range of 1000 to 3000cp, the molecular weight is 600 to 900, and the curing yield of the ceramic is more than 60 percent.
Further, in the step 4), N is adopted 2 Pressurizing under the atmosphere, wherein the pressure of the pressurized impregnation is 1-2 MPa, and the impregnation time is 4-6h.
Further, in the step 5), performing crosslinking curing on the PBSZ polymer precursor, wherein the temperature of the crosslinking curing is 170-300 ℃, and the curing time is 2-4 h; the cracking temperature is 1000-1200 ℃ and the time is 2-4 h.
Further, the density of the C/PyC-SiC-HfC/C-SiBCN composite material is 1.7-1.9g/cm 3 The porosity is 4-5vol%.
Advantageous effects
The invention adopts a three-interface phase complementary high-temperature resistant system of PyC-SiC-HfC, utilizes the good lamellar structure of PyC, the good ablation resistance of HfC and the good thermal expansion coefficient matching capability of SiC as the interface phase of the C/C-SiBCN composite material so as to improve the ablation resistance of the whole composite material, and the density of the prepared C/PyC-SiC-HfC/C-SiBCN composite material reaches 1.7-1.9g/cm 3 The porosity is 4-5vol%.
Drawings
FIG. 1 is a schematic flow chart of the present invention
FIG. 2 is a schematic view of the microstructure of the ablated central region of the present invention
Detailed Description
The following description is provided for illustrative purposes and is not intended to limit the invention to the particular embodiments disclosed.
Example 1:
a PyC-SiC-HfC three-interface phase modified C/C-SiBCN double-matrix ablation-resistant composite material is shown in a reference figure 1, and the preparation method comprises the following steps:
preparing a pyrolytic carbon interface phase and a silicon carbide interface phase: placing the cut 2D carbon felt in a graphite mold in a laminated mode, then placing the mold in a chemical reaction deposition furnace, and setting specific parameters as follows: pressure: 100mbar; residence time of gas in the mold: 0.5s; temperature: 965 deg.C. The gas flow rate is calculated from the residence time, deposition temperature and pressure correlation by:
when pyrolytic carbon is deposited for 90min under the parameters, a PyC interface layer with the thickness of about 250nm can be prepared on the surface of the sample.
Placing a prefabricated body of the prepared PyC interface layer in a mould, placing the mould in a deposition position in a gas deposition furnace, and using a gas source with a gas component of MTS-H2-N2 as a reaction precursor system, wherein the detailed interface preparation parameters are as follows: gas ratio: MTS (methyltrichlorosilane): h2: n2= 1; temperature: 1050 ℃; pressure: 100mbar, residence time of gas in the mould: 0.5s; and then calculating and measuring the residual volume of the relevant used mold, calculating by using a formula (1) to obtain the total gas flow, and then calculating the relevant gas flow according to the proportional relation.
Preparing a hafnium carbide interface phase: and measuring the volume and the mass of the preform, obtaining the density of the composite material according to the Archimedes drainage method, and selecting a hafnium carbide interface with the designed mass fraction of 13%. And (3) using an impregnation cracking process, placing the carbon fiber preform deposited with the double interfaces in a hafnium carbide impregnation liquid for impregnation for 2h, placing the carbon fiber preform impregnated with the hafnium carbide impregnation liquid in a tubular furnace, heating to 1500 ℃ so that the impregnation liquid is converted into hafnium carbide crystals, and calculating the mass change. And then the process is circulated for many times, so that the mass fraction of the impregnation reaches 13 percent.
Preparing a carbon matrix by a CVI process: through earlier calculation, the SiBCN matrix can keep the continuity when the density of the C matrix reaches 1.3 percent or below, and the carbon matrix density is designed to ensure that the SiBCN matrix is continuousThe degree is 1.25g/cm 3 . The carbon source and the preparation method of the C matrix are similar to those of the PyC interface, and C is adopted 3 H 6 As a carbon source for reaction, the deposition pressure is 100mbar, the gas retention time is 0.5s, and the deposition time is set to be 12h to prepare a compact composite material, wherein the density of a preform obtained by deposition is about 1.3g/cm 3 To achieve a predetermined preform density.
PIP preparation of SiBCN matrix: cutting the composite material deposited with the C matrix into a preset shape, placing the composite material in a pressure reaction kettle, externally connecting a vacuum pump to dry air in the kettle, adding PBSZ into the reaction kettle until the sample is completely impregnated, and adopting N to improve the impregnation efficiency 2 Pressurizing under the atmosphere, wherein the applied pressure is 1MPa, and the impregnation time is 4h, so as to obtain a C/SiBCN composite material green body; and secondly, carrying out crosslinking and curing on the PBSZ polymer precursor: utilizing a heating device of the pressure reaction kettle to raise the temperature in the kettle to 170 ℃ (the pressure of the whole system is still kept at 1 MPa), setting the curing time to be 2h, closing the heating device, and cooling the sample to room temperature along with the reaction kettle; and finally carrying out a ceramic transformation process: taking out the sample from the kettle, transferring the sample into a high-temperature tube furnace, and performing ceramization at 1000 ℃ under the protective atmosphere of N for pyrolysis ceramization 2 The time is 2h. This procedure was repeated 5 times to obtain a denser composite material (density 1.87 g/cm) 3 Porosity 4.75 vol%).
Oxyacetylene ablation experiments: the oxyacetylene flame ablated the composite material for 60 seconds, and the measured line ablation rate was only 2 μm/s. The ablated central region microstructure is shown in figure 2.
Comparative example 1:
the preparation process is similar to the above, except that the hafnium carbide interface phase is not prepared, namely the prepared material is a PyC-SiC double-interface phase modified C/C-SiBCN double-matrix ablation-resistant material. The density of the composite material finally prepared by the experiment is 1.81g/cm 3 Porosity 5.42vol%.
The wire ablation rate is 31 mu m/s after being ablated for 60s by the oxyacetylene flame.
Comparative example 2:
the preparation process is similar to the above, notAnd preparing a SiBCN matrix phase, and using a C matrix phase, namely preparing the material which is a PyC-SiC-HfC three-interface phase modified C/C composite material. The density of the composite material finally prepared by the experiment is 1.72g/cm 3 And the porosity is 6.21vol%.
The wire ablation rate is 19 mu m/s after being ablated for 60s by the oxyacetylene flame.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The preparation method of the PyC-SiC-HfC three-interface phase modified C/C-SiBCN double-matrix ablation-resistant composite material is characterized by comprising the preparation of a PyC-SiC-HfC interface phase and a C-SiBCN matrix, and specifically comprises the following steps: (1) Preparing a PyC + SiC interface phase on the fiber surface of the carbon fiber preform by using a CVD (chemical vapor deposition) process to obtain a preform with an interface phase with a certain thickness; (2) Dipping the prefabricated body prepared in the step (1) in an HfC polymer-xylene solution for multiple times to prepare a PyC-SiC-HfC three-interface phase modified carbon fiber prefabricated body material; (3) preparing a C matrix by a CVI process; (4) preparing a SiBCN modified matrix through a PIP process; (5) curing and cracking; (6) And (5) repeating the steps (4) and (5) to finally obtain the C/PyC-SiC-HfC/C-SiBCN composite material.
2. The production method according to claim 1, wherein the carbon fiber preform is a 2D laminated carbon fiber.
3. The method of claim 1, wherein the carbon source selected for PyC interface deposition is C 3 H 6 Or CH 4 The deposition pressure of alkane gas is 10-20KPa, the deposition time is 10-15h, the deposition temperature is 950-1000 ℃, and the residence time of deposition is 0.5-1s.
4. The method of claim 1, wherein S is deposited as selectedThe gas source of the iC interface is MTS + H 2 +N 2 The deposition pressure is 10-20KPa, the temperature is 1050 ℃, and the deposition time is 12-15h.
5. The method as claimed in claim 1, wherein the immersion in the HfC polymer-xylene solution in step 2) is carried out for a period of 2 to 5 hours at an immersion mass fraction of 13 to 15, and the heat treatment temperature used is 1500 to 1600 ℃ depending on the temperature at which the hafnium carbide crystals are formed.
6. The method according to claim 1, wherein the carbon matrix density is designed to be 1.2 to 1.4g/cm in the step 3) 3 The selected gas source is CH 4 Or C 3 H 6 The deposition pressure of alkane gas is 100-200mbar, the gas retention time is 0.5-1s, and the deposition time is 10-14h.
7. The method of claim 1, wherein in step 4), the polyborosilazane precursor has a boron content of between 1-2%, a viscosity in the range of 1000-3000cp, a molecular weight of 600-900, and a ceramic cure yield of >60%.
8. The method according to claim 1, wherein in the step 4), N is used 2 Pressurizing in atmosphere, wherein the pressure of the pressurized impregnation is 1-2 MPa, and the impregnation time is 4-6h.
9. The preparation method according to claim 1, wherein in the step 5), the PBSZ polymer precursor is subjected to crosslinking and curing, wherein the crosslinking and curing temperature is 170-300 ℃, and the curing time is 2-4 h; the cracking temperature is 1000-1200 ℃ and the time is 2-4 h.
10. The method according to claim 1, wherein the C/PyC-SiC-HfC/C-SiBCN composite material has a density of 1.7 to 1.9g/cm 3 The porosity is 4-5vol%.
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| CN117003572A (en) * | 2023-08-01 | 2023-11-07 | 上海大学 | Preparation method of deposition PyC/SiC interface phase and ceramic matrix composite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109970460A (en) * | 2018-11-23 | 2019-07-05 | 中国科学院金属研究所 | A kind of fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material and preparation method thereof |
| CN112299865A (en) * | 2020-11-19 | 2021-02-02 | 航天特种材料及工艺技术研究所 | Modified C/SiC composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109970460A (en) * | 2018-11-23 | 2019-07-05 | 中国科学院金属研究所 | A kind of fibre reinforced (carbon -) is silicon carbide-based-ultra-temperature ceramic-based composite material and preparation method thereof |
| CN112299865A (en) * | 2020-11-19 | 2021-02-02 | 航天特种材料及工艺技术研究所 | Modified C/SiC composite material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117003572A (en) * | 2023-08-01 | 2023-11-07 | 上海大学 | Preparation method of deposition PyC/SiC interface phase and ceramic matrix composite |
| CN117003572B (en) * | 2023-08-01 | 2024-05-07 | 上海大学 | Preparation method of deposition PyC/SiC interface phase and ceramic matrix composite |
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