CN114230347A - Preparation method and product of continuous fiber reinforced ZrC/SiC composite part - Google Patents
Preparation method and product of continuous fiber reinforced ZrC/SiC composite part Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 121
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 116
- 238000000197 pyrolysis Methods 0.000 claims abstract description 44
- 238000003763 carbonization Methods 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000005011 phenolic resin Substances 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 35
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 34
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 30
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 28
- 239000004917 carbon fiber Substances 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 25
- 239000011241 protective layer Substances 0.000 claims abstract description 24
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229920005989 resin Polymers 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 20
- 239000000654 additive Substances 0.000 claims abstract description 18
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 239000002296 pyrolytic carbon Substances 0.000 claims abstract description 11
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 69
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 66
- 238000000151 deposition Methods 0.000 claims description 17
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 15
- 230000008021 deposition Effects 0.000 claims description 14
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- 238000001764 infiltration Methods 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 11
- 229910052726 zirconium Inorganic materials 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 10
- 238000005336 cracking Methods 0.000 claims description 9
- 229920002748 Basalt fiber Polymers 0.000 claims description 8
- 239000003365 glass fiber Substances 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 6
- 239000011863 silicon-based powder Substances 0.000 claims description 6
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 5
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- 239000004417 polycarbonate Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 238000003475 lamination Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 229910007735 Zr—Si Inorganic materials 0.000 abstract description 31
- 238000005516 engineering process Methods 0.000 abstract description 10
- 239000011153 ceramic matrix composite Substances 0.000 abstract description 2
- 238000010000 carbonizing Methods 0.000 abstract 1
- 229910026551 ZrC Inorganic materials 0.000 description 49
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 46
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
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- 239000005055 methyl trichlorosilane Substances 0.000 description 4
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 4
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 229910021431 alpha silicon carbide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- NQKXFODBPINZFK-UHFFFAOYSA-N dioxotantalum Chemical compound O=[Ta]=O NQKXFODBPINZFK-UHFFFAOYSA-N 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
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Abstract
The invention belongs to the technical field related to high-temperature ceramic matrix composites, and discloses a preparation method and a product of a continuous fiber reinforced ZrC/SiC composite part. The method comprises the following specific steps: s1, preparing a continuous fiber reinforced resin primary blank by adopting an additive manufacturing technology; s2, carrying out pyrolysis carbonization on the primary blank to obtain a carbon primary blank; s3, generating a protective layer on the surface of the carbon fiber in the prepared carbon primary blank to protect the continuous fiber; s4, impregnating the carbon primary blank in a thermosetting phenolic resin solution, curing, and then pyrolyzing and carbonizing again to densify; s5 repeating the step S4 for multiple times to obtain a final carbon preform, and carrying out Zr-Si reaction sintering on the carbon preform to enable pyrolytic carbon in the carbon preform to react with Zr-Si to generate ZrC-SiC, so that the continuous fiber reinforced ZrC/SiC composite part is obtained. By the method, the problems that the SiC product cannot resist high temperature and the component structure in the carbon fiber reinforced ZrC is not uniformly distributed are solved.
Description
Technical Field
The invention belongs to the technical field of high-temperature ceramic matrix composite materials, and particularly relates to a preparation method and a product of a continuous fiber reinforced ZrC/SiC composite part.
Background
The ZrC ceramic has high melting point (3540 ℃), high strength, high hardness and good thermal shock resistance. Meanwhile, in a high-temperature oxidation environment, the oxidation product ZrO2Not only has high melting point (2770 ℃ higher than HfO)2And TaO2) And has relatively low vapor pressure and thermal conductivity, are desirable high temperature ceramic materials. In addition, ZrC has a lower density than HfC, TaC,the price is cheaper, and the light weight requirement in aerospace application is better met. SiC has high specific strength and specific modulus, and has a thermal expansion coefficient which is not much different from that of a carbon matrix (the alpha-SiC is 3.8-5.2 e)-6Temperature/° C, pyrolytic carbon (PyC) 1.0-2.0e-6The temperature per DEG C) can effectively relieve the problem of the thermal expansion coefficient adaptability of the composite material in the preparation and use processes. Therefore, the prepared continuous fiber reinforced ZrC/SiC composite material has higher ablation resistance, and simultaneously, the fiber can reinforce and toughen the ceramic matrix, so that the prepared ZrC/SiC composite material part has excellent mechanical properties.
The ZrC/SiC composite material is a necessary material for a high-speed aircraft protection system, an aircraft engine hot end part, a high-performance brake system and the like due to the properties of low density, high strength, oxidation resistance, ablation erosion resistance and the like. The traditional method is difficult to form large ceramic parts with complex structures, and some complex parts can not be integrally formed. The additive manufacturing technology adopts a mode of manufacturing layer by layer and overlapping, is very suitable for forming parts with complex structures, but has high melting temperature and large brittleness of ceramics, and can be directly melted by laser, so that the obtained parts have large stress and are easy to have cracks.
CN201510881857.3 discloses a carbon fiber reinforced zirconium carbide composite material and a preparation method thereof, wherein a carbon fiber preform is adopted as a reinforcement, and then a vacuum impregnation zirconium source and a cross-linking solidification zirconium source are repeatedly adopted to prepare the carbon fiber reinforced zirconium carbide composite material. Firstly, the carbon fiber preform adopted by the method is in a fixed shape, and a part is prepared by adopting a machining process in the later period, so that the process is complex; secondly, the method adopts a vacuum impregnation zirconium source and a cross-linking solidification zirconium source, the impregnation depth of the zirconium source is shallow, and the uniform distribution of the component structure of the material cannot be realized. CN201910874219.7 discloses a method for preparing a carbon fiber-zirconium carbide composite material, which comprises immersing a carbon fiber woven body coated with zirconium carbide in a zirconium carbide precursor sol, drying in a vacuum drying oven, and then putting into a sintering furnace to crack in an inert gas atmosphere to obtain the carbon fiber-zirconium carbide composite material. The method still faces the problems that parts need to be processed and formed in the later period, and the carbon fiber-zirconium carbide composite material is uneven in component structure due to uneven impregnation of zirconium carbide precursor sol. CN201910684009.1 discloses a continuous fiber reinforced SiC part preparation method and product based on additive manufacturing, the method adopts additive manufacturing to prepare a primary blank, prepares a carbon preform through pyrolysis and carbonization, and prepares a continuous fiber reinforced SiC part through reaction sintering, the SiC part prepared by the method is a SiC part, and the SiC part cannot be used in a high-temperature environment.
Disclosure of Invention
Aiming at the defects or improvement requirements in the prior art, the invention provides a preparation method and a product of a continuous fiber reinforced ZrC/SiC composite part, which solve the problems that a SiC product cannot resist high temperature and the component structure in carbon fiber reinforced zirconium carbide is not uniformly distributed.
To achieve the above object, according to one aspect of the present invention, there is provided a method for producing a continuous fiber-reinforced ZrC/SiC composite part, the method comprising the steps of:
s1, according to the three-dimensional structure of the ZrC/SiC composite part to be formed, using continuous fibers and a binder as raw materials to perform additive manufacturing, so as to obtain a continuous fiber reinforced resin primary blank;
s2, carrying out pyrolysis carbonization on the resin primary blank to obtain a carbon primary blank, wherein in the pyrolysis carbonization process, the resin in the resin primary blank is pyrolyzed and carbonized to form carbon, and meanwhile, the volume of the resin primary blank is shrunk to form air holes;
s3, carrying out chemical vapor infiltration or precursor impregnation cracking on the carbon primary blank by using an organic Sr source, so as to form a ZrC protective layer on the surface of continuous fibers in the carbon primary blank;
s4 impregnating the carbon preform subjected to the step S3 in a thermosetting phenolic resin solution so that the thermosetting phenolic resin impregnates the pores of the carbon preform, curing the impregnated carbon preform, and then performing pyrolysis carbonization again to obtain a carbon preform;
and S5, reacting and sintering the carbon preform together with the mixed powder of silicon powder and zirconium powder, wherein the pyrolytic carbon in the carbon preform reacts with the silicon and the zirconium to generate ZrC-SiC, so that the ZrC/SiC composite part reinforced by the continuous fiber is obtained.
Further preferably, in step S1, the continuous carbon fibers are one or more of continuous carbon fibers, continuous silicon carbide fibers, continuous glass fibers and continuous basalt fibers, and the binder is one or more of phenolic resin, epoxy resin, polylactic acid and polycarbonate.
Further preferably, in step S2, the temperature of the pyrolysis carbonization is 600 ℃ to 900 ℃ and the time is 0.5h to 3 h.
Further preferably, in step S3, the thickness of the protective layer formed on the surface of the continuous fiber by the chemical vapor infiltration or the precursor impregnation and pyrolysis is 1nm to 100 nm. Further preferably, the step S4 is repeated a plurality of times, thereby further increasing the density of carbon in the carbon preform.
More preferably, in step S4, the thermosetting phenol resin has a carbon residue ratio of 40% to 50%.
Further preferably, in step S5, the reaction sintering temperature is 1700 ℃ to 2300 ℃ and the time is 1h to 10 h.
Further preferably, in step S5, the content of silicon powder in the mixed powder of silicon powder and zirconium powder is not more than 10%.
Further preferably, in step S1, the additive manufacturing is performed by fused deposition modeling, directed energy deposition, or thin-material lamination.
According to another aspect of the invention, a continuous fiber reinforced ZrC/SiC composite part product prepared by the preparation method is provided.
Generally, compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1. according to the method, zirconium is added into continuous fiber silicon carbide to obtain the ZrC/SiC composite part, wherein the melting point of zirconium element is high, the ZrC composite part is different from the existing ceramic material and cannot be used at high temperature for a long time, ZrC can be used at the temperature of more than 2000 ℃ for a long time, and the ZrC composite part has excellent high temperature resistance, has lower density and lower price, and is more suitable for light weight requirement performance in aerospace application;
2. in the invention, in step S3, a ZrC protective layer is formed on the surface of the continuous fiber by using an organic zirconium source, so that the reaction between carbon in the continuous fiber and silicon or zirconium is avoided in the reaction sintering process, and pyrolytic carbon is used for reacting with Zr-Si in the reaction sintering process, so that the continuous fiber in the part is protected, and the weakening of the reinforcing effect of the continuous fiber is avoided;
3. in the invention, the pyrolytic carbonization is carried out in the step S2, the density of the prepared pyrolytic carbon is low and is not enough to react with Zr/Si to generate a compact ceramic material, so that the pyrolytic carbon is infiltrated and pyrolytic carbonized for multiple times in the step S4, the density of the pyrolytic carbon is increased, and the pyrolytic carbon reacts with Zr/Si to generate the compact ceramic material, so that the prepared part has excellent performance;
4. the invention adopts the repeated infiltration-carbonization process, so that carbon can be fully and uniformly covered on the surface of the continuous fiber, stable and uniform ZrC/SiC can be generated on the surface of the original continuous fiber in the subsequent reaction sintering reaction, and the intermediate infiltration process can make up the gap between the carbon obtained by the first carbonization and the ZrC/SiC;
5. according to the ZrC/SiC composite part prepared by the method, continuous fibers are formed by an additive manufacturing technology, and the arrangement and orientation of the fibers can be regulated and controlled according to design requirements, so that the components of the prepared part are uniformly distributed, and the performance of the part is improved.
Drawings
FIG. 1 is a flow chart of a method of making and forming a continuous fiber reinforced ZrC/SiC composite constructed in accordance with a preferred embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in FIG. 1, the preparation method of the continuous fiber reinforced ZrC/SiC composite part comprises the following steps:
(a) forming a continuous fiber composite resin primary blank by adopting a continuous fiber additive manufacturing technology according to the three-dimensional structure of the ZrC/SiC composite part to be formed;
in step (a), the continuous fibers are preferably continuous carbon fibers, continuous silicon carbide fibers, continuous glass fibers, or continuous basalt fibers.
In step (a), the additive manufacturing technique is preferably Fused Deposition Modeling (FDM), Directed Energy Deposition (DED), thin layer stack (LOM).
In the step (a), the binder is one or more of phenolic resin, epoxy resin, polylactic acid and polycarbonate.
(b) Performing pyrolysis carbonization on the resin primary blank to obtain a carbon primary blank, wherein in the pyrolysis carbonization process, the resin in the primary blank is pyrolyzed and carbonized to form carbon, so that the volume of the carbon primary blank is shrunk to form air holes on one hand, and the resin in the primary blank is carbonized on the other hand;
in the step (b), the pyrolysis carbonization temperature is 600-900 ℃, the time is 0.5-3 h, the carbonization starts at the temperature of more than 600 ℃ of the binder, and the carbonization product is ensured to be amorphous cracked carbon at the temperature of less than 900 ℃.
(c) Generating a protective layer on the surface of the continuous fiber in the prepared carbon primary blank by adopting a Chemical Vapor Infiltration (CVI) or a precursor impregnation pyrolysis method (PIP) to protect the continuous fiber;
in the step (c), the thickness of the protective layer generated on the surface of the continuous fiber by chemical vapor infiltration or precursor impregnation and pyrolysis is 1 nm-100 nm.
(d) Impregnating a carbon primary blank in a thermosetting phenolic resin solution, so that the thermosetting phenolic resin is impregnated into pores of the carbon primary blank, curing the impregnated carbon primary blank, and then performing pyrolysis carbonization again, wherein in the pyrolysis carbonization process, the carbon content in the preform is further increased through the pyrolysis carbonization of the thermosetting phenolic resin;
in the step (d), the carbon residue rate of the thermosetting phenolic resin is preferably 40-50%, and experiments prove that the phenolic resin with the carbon residue rate of 40-50% has uniform pores in the carbonization process, thereby being beneficial to multiple infiltration-pyrolysis carbonization densification.
(e) And (d) repeating the step (d) for multiple times to obtain a final carbon preform, and carrying out Zr-Si reaction sintering on the final carbon preform to enable pyrolytic carbon in the final carbon preform to react with Zr-Si to generate ZrC-SiC, so as to obtain the continuous fiber reinforced ZrC/SiC composite material part.
In the step (e), repeating the step (d) for multiple times, wherein the number of the repeated times is determined according to the density and the structure of the ZrC/SiC composite material part finally required.
In the step (e), the content of Si in the Zr-Si reaction sintering is 0-10%, the Si is added to increase the infiltration of Zr so that the reaction sintering can be fully carried out, the addition of 0 is pure Zr, the reaction sintering thickness is thinner, and the Zr-Si reaction sintering method is suitable for thin-wall structural parts. The reason why the Si content is less than 10% is that if the Si content is further increased, the high temperature performance of the part is affected by the increase of the produced SiC. .
In the step (e), the reaction sintering temperature is 1700 ℃ to 2300 ℃, and the temperature is determined according to different melting points of Zr-Si content proportions; the time is 1-10 h, and the reaction time is determined according to the size and the wall thickness of the part.
In summary, the general idea of the present invention mainly includes five aspects, one is to establish a CAD model based on design requirements and prepare a preform by a continuous fiber additive manufacturing technique; secondly, the prepared primary blank is pyrolyzed and carbonized; thirdly, forming a protective layer on the surface of the continuous fiber by adopting a CVI (chemical vapor infiltration) or PIP (Poly-propylene-oxide-polyester) process; fourthly, repeatedly impregnating the thermosetting phenolic resin solution with high carbon residue rate, and improving the carbon density by adopting a pyrolysis carbonization process; fifthly, carrying out Zr-Si reaction sintering process treatment on the prefabricated body subjected to multiple carbonization treatment to obtain the ZrC/SiC composite material part.
The invention will now be further illustrated with reference to specific examples.
Example 1
(1) Designing a CAD model of the ZrC/SiC composite part, and forming continuous carbon fibers by adopting a fused deposition additive manufacturing technology to prepare a continuous carbon fiber composite resin primary blank, wherein the resin is polylactic acid;
(2) carrying out pyrolysis carbonization on the continuous carbon fiber composite resin primary blank to obtain a carbon primary blank, wherein the pyrolysis carbonization temperature is 600 ℃, and the time is 1 h;
(3) generating a protective layer on the surface of continuous carbon fibers in the prepared carbon primary blank by adopting Chemical Vapor Infiltration (CVI) to protect the continuous fibers, taking methyltrichlorosilane as a silicon source, placing the carbon primary blank in a deposition furnace, heating to 1100 ℃, conveying pyrolysis gas containing the silicon source generated after pyrolysis of the methyltrichlorosilane at high temperature to the periphery of a carbon preform by a pressure difference method, depositing for 0.5h, and forming a SiC protective layer on the surface of the continuous carbon fibers, wherein the thickness of the SiC protective layer is 1 nm;
(4) impregnating a carbon primary blank in a thermosetting phenolic resin solution, wherein the residual carbon rate of the thermosetting phenolic resin is 40%, so that the thermosetting phenolic resin is impregnated into the pores of the carbon primary blank, curing the impregnated carbon primary blank, then performing pyrolysis carbonization again, and repeating the step (4) for multiple times to obtain a final carbon preform;
(5) and performing Zr-Si reaction sintering on the final carbon preform, wherein the content of Si in the Zr-Si reaction sintering is 10%, placing the repeatedly carbonized part and Zr-Si particles in a vacuum furnace, vacuumizing and heating to 1900 ℃, preserving heat for 1h, and performing reaction sintering on the preform and liquid Zr-Si to generate ZrC-SiC, thereby obtaining the continuous fiber reinforced ZrC/SiC composite material part.
Example 2
(1) Designing a CAD model of a ZrC/SiC composite part, and forming continuous carbon fibers by adopting a fused deposition additive manufacturing technology to prepare a continuous carbon fiber composite resin primary blank, wherein the resin is polycarbonate;
(2) carrying out pyrolysis carbonization on the continuous carbon fiber composite resin primary blank to obtain a carbon primary blank, wherein the pyrolysis carbonization temperature is 900 ℃, and the time is 3 hours;
(3) generating a protective layer on the surface of continuous carbon fibers in the prepared carbon primary blank by adopting Chemical Vapor Infiltration (CVI) to protect the continuous fibers, taking methyltrichlorosilane as a silicon source, placing the carbon primary blank in a deposition furnace, heating to 1100 ℃, conveying pyrolysis gas containing the silicon source generated after pyrolysis of the methyltrichlorosilane at high temperature to the periphery of a carbon preform by a pressure difference method, depositing for 5 hours, and forming a SiC protective layer on the surface of the continuous carbon fibers, wherein the thickness of the SiC protective layer is 100 nm;
(4) impregnating the carbon primary blank in a thermosetting phenolic resin solution, wherein the residual carbon rate of the thermosetting phenolic resin is 50%, so that the thermosetting phenolic resin is impregnated into the pores of the carbon primary blank, curing the impregnated carbon primary blank, and repeating the step (4) for multiple times to obtain a final carbon preform;
(5) and performing Zr-Si reaction sintering on the final carbon preform, wherein Si is not contained in the Zr-Si reaction sintering, namely the content of Si is 0%, placing the repeatedly carbonized part and Zr particles in a vacuum furnace, vacuumizing and heating to 2300 ℃, preserving heat for 10h, and performing reaction sintering on the preform and liquid Zr to generate ZrC, thereby obtaining the continuous fiber reinforced ZrC composite part.
Example 3
(1) Designing a CAD model of the ZrC/SiC composite part, and forming continuous silicon carbide fiber by adopting a directional energy deposition additive manufacturing technology to prepare a continuous silicon carbide fiber composite resin primary blank, wherein the resin is epoxy resin;
(2) carrying out pyrolysis carbonization on the continuous silicon carbide fiber composite resin primary blank to obtain a carbon primary blank, wherein the pyrolysis carbonization temperature is 800 ℃, and the time is 2 hours;
(3) generating a protective layer on the surface of continuous silicon carbide fiber in the prepared carbon primary blank by adopting a precursor impregnation pyrolysis process (PIP) to protect the continuous fiber, vacuumizing to remove air in the carbon primary blank, then soaking the carbon primary blank into a toluene solution of polycarbosilane, pressurizing to fully fill pores of the carbon primary blank with the polycarbosilane, after curing, moving the carbon primary blank filled with the polycarbosilane into a cracking furnace, carrying out heat treatment at 900 ℃ under a vacuum condition, and carrying out high-temperature cracking on the polycarbosilane to form a SiC protective layer on the surface of the continuous silicon carbide fiber, wherein the thickness is 10 nm;
(4) impregnating a carbon primary blank in a thermosetting phenolic resin solution, wherein the residual carbon rate of the thermosetting phenolic resin is 40%, so that the thermosetting phenolic resin is impregnated into the pores of the carbon primary blank, curing the impregnated carbon primary blank, then performing pyrolysis carbonization again, and repeating the step (4) for multiple times to obtain a final carbon preform;
(5) and performing Zr-Si reaction sintering on the final carbon preform, wherein the content of Si in the Zr-Si reaction sintering is 5%, placing the repeatedly carbonized part and Zr-Si particles in a vacuum furnace, vacuumizing and heating to 1800 ℃, preserving heat for 1h, and performing reaction sintering on the preform and liquid Zr-Si to generate ZrC-SiC, thereby obtaining the continuous fiber reinforced ZrC/SiC composite material part.
Example 4
(1) Designing a CAD model of the ZrC/SiC composite part, and forming continuous carbon fibers by adopting a thin material lamination additive manufacturing technology to prepare a continuous carbon fiber composite resin primary blank, wherein the resin is phenolic resin;
(2) carrying out pyrolysis carbonization on the continuous carbon fiber composite resin primary blank to obtain a carbon primary blank, wherein the pyrolysis carbonization temperature is 700 ℃, and the time is 3 h;
(3) generating a protective layer on the surface of continuous carbon fibers in the prepared carbon primary blank by adopting Chemical Vapor Infiltration (CVI) to protect the continuous fibers, taking methane as a carbon source, placing the carbon primary blank in a deposition furnace, heating to 1000 ℃, conveying the methane gas to the periphery of a carbon preform, depositing for 2 hours, and forming a deposited C protective layer on the surface of the continuous carbon fibers, wherein the thickness of the deposited C protective layer is 100 nm;
(4) impregnating a carbon primary blank in a thermosetting phenolic resin solution, wherein the residual carbon rate of the thermosetting phenolic resin is 45%, so that the thermosetting phenolic resin is impregnated into the pores of the carbon primary blank, curing the impregnated carbon primary blank, then performing pyrolysis carbonization again, and repeating the step (4) for multiple times to obtain a final carbon preform;
(5) and performing Zr-Si reaction sintering on the final carbon preform, wherein the content of Si in the Zr-Si reaction sintering is 3%, placing the repeatedly carbonized part and Zr-Si particles in a vacuum furnace, vacuumizing and heating to 1900 ℃, preserving the temperature for 5h, and performing reaction sintering on the preform and liquid Zr-Si to generate ZrC-SiC, thereby obtaining the continuous fiber reinforced ZrC/SiC composite material part.
Example 5
(1) Designing a CAD model of the ZrC/SiC composite part, and forming continuous glass fibers by adopting a fused deposition modeling additive manufacturing technology to prepare a continuous glass fiber composite resin primary blank, wherein the resin is polylactic acid;
(2) carrying out pyrolysis carbonization on the continuous glass fiber composite resin primary blank to obtain a carbon primary blank, wherein the pyrolysis carbonization temperature is 900 ℃, and the time is 0.5 h;
(3) generating a protective layer on the surface of continuous glass fiber in the prepared carbon primary blank by adopting a precursor impregnation pyrolysis process (PIP) to protect the continuous fiber, vacuumizing to remove air in the preform, then soaking the preform in a toluene solution of polycarbosilane, pressurizing to fully fill pores of the carbon primary blank with the polycarbosilane, curing, then transferring the carbon primary blank filled with the polycarbosilane into a cracking furnace, carrying out heat treatment at 1000 ℃ under a vacuum condition, and carrying out high-temperature cracking on the polycarbosilane to form a SiC protective layer on the surface of the continuous glass fiber, wherein the thickness is 50 nm;
(4) impregnating a carbon primary blank in a thermosetting phenolic resin solution, wherein the residual carbon rate of the thermosetting phenolic resin is 40%, so that the thermosetting phenolic resin is impregnated into the pores of the carbon primary blank, curing the impregnated carbon primary blank, then performing pyrolysis carbonization again, and repeating the step (4) for multiple times to obtain a final carbon preform;
(5) and performing Zr-Si reaction sintering on the final carbon preform, wherein the content of Si in the Zr-Si reaction sintering is 6%, placing the repeatedly carbonized part and Zr-Si particles in a vacuum furnace, vacuumizing and heating to 1700 ℃, preserving heat for 3h, and performing reaction sintering on the preform and liquid Zr-Si to generate ZrC-SiC, thereby obtaining the continuous fiber reinforced ZrC/SiC composite material part.
Example 6
(1) Designing a CAD model of a ZrC/SiC composite part, and forming continuous basalt fiber by adopting a directional energy deposition additive manufacturing technology to prepare a continuous basalt fiber composite resin primary blank, wherein the resin is phenolic resin;
(2) carrying out pyrolysis carbonization on the continuous basalt fiber composite resin primary blank to obtain a carbon primary blank, wherein the pyrolysis carbonization temperature is 600 ℃, and the time is 3 h;
(3) generating a protective layer on the surface of continuous basalt fiber in the prepared carbon primary blank by adopting a precursor impregnation pyrolysis process (PIP) to protect the continuous fiber, vacuumizing to remove air in the carbon primary blank, then soaking the carbon primary blank into a toluene solution of polycarbosilane, pressurizing to fully fill pores of the carbon primary blank with the polycarbosilane, curing, then transferring the carbon primary blank filled with the polycarbosilane into a cracking furnace, carrying out heat treatment at 950 ℃ under a vacuum condition, and carrying out high-temperature cracking on the polycarbosilane to form a SiC protective layer on the surface of the continuous basalt fiber, wherein the thickness is 80 nm;
(4) impregnating a carbon primary blank in a thermosetting phenolic resin solution, wherein the residual carbon rate of the thermosetting phenolic resin is 43 percent, so that the thermosetting phenolic resin is impregnated into the pores of the carbon primary blank, curing the impregnated carbon primary blank, then performing pyrolysis carbonization again, and repeating the step (4) for multiple times to obtain a final carbon preform;
(5) and performing Zr-Si reaction sintering on the final carbon preform, wherein the content of Si in the Zr-Si reaction sintering is 8%, placing the repeatedly carbonized part and Zr-Si particles in a vacuum furnace, vacuumizing and heating to 1700 ℃, preserving heat for 2h, and performing reaction sintering on the preform and liquid Zr-Si to generate ZrC-SiC, thereby obtaining the continuous fiber reinforced ZrC/SiC composite material part.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a continuous fiber reinforced ZrC/SiC composite part is characterized by comprising the following steps:
s1, according to the three-dimensional structure of the ZrC/SiC composite part to be formed, using continuous fibers and a binder as raw materials to perform additive manufacturing, so as to obtain a continuous fiber reinforced resin primary blank;
s2, carrying out pyrolysis carbonization on the resin primary blank to obtain a carbon primary blank, wherein in the pyrolysis carbonization process, the resin in the resin primary blank is pyrolyzed and carbonized to form carbon, and meanwhile, the volume of the resin primary blank is shrunk to form air holes;
s3, carrying out chemical vapor infiltration or precursor impregnation cracking on the carbon primary blank by using an organic Sr source, so as to form a ZrC protective layer on the surface of continuous fibers in the carbon primary blank;
s4 impregnating the carbon preform subjected to the step S3 in a thermosetting phenolic resin solution so that the thermosetting phenolic resin impregnates the pores of the carbon preform, curing the impregnated carbon preform, and then performing pyrolysis carbonization again to obtain a carbon preform;
and S5, reacting and sintering the carbon preform together with the mixed powder of silicon powder and zirconium powder, wherein the pyrolytic carbon in the carbon preform reacts with the silicon and the zirconium to generate ZrC-SiC, so that the ZrC/SiC composite part reinforced by the continuous fiber is obtained.
2. The method of claim 1, wherein in step S1, the continuous carbon fiber is one or more of continuous carbon fiber, continuous silicon carbide fiber, continuous glass fiber and continuous basalt fiber, and the binder is one or more of phenolic resin, epoxy resin, polylactic acid and polycarbonate.
3. The method for producing a continuous fiber-reinforced ZrC/SiC composite part according to claim 1 or 2, wherein in step S2, the temperature of the pyrolytic carbonization is 600 ℃ to 900 ℃ for 0.5h to 3 h.
4. The method for producing a continuous fiber-reinforced ZrC/SiC composite part according to claim 1 or 2, wherein in step S3, the thickness of the protective layer formed on the surface of the continuous fiber by chemical vapor infiltration or precursor impregnation cracking is 1nm to 100 nm.
5. The method of producing a continuous fiber-reinforced ZrC/SiC composite part according to claim 1 or 2, wherein step S4 is repeated a plurality of times to further increase the density of carbon in the carbon preform.
6. The method of producing a continuous fiber-reinforced ZrC/SiC composite part according to claim 1 or 2, wherein in step S4, the carbon residue ratio of the thermosetting phenol resin is 40% to 50%.
7. The method for producing a continuous fiber-reinforced ZrC/SiC composite part as set forth in claim 1 or 2, wherein the temperature of the reaction sintering is 1700 ℃ to 2300 ℃ for 1h to 10h in step S5.
8. The method of producing a continuous fiber-reinforced ZrC/SiC composite part according to claim 1 or 2, wherein in step S5, the content of silicon powder in the mixed powder of silicon powder and zirconium powder does not exceed 10%.
9. A method of making a continuous fiber reinforced ZrC/SiC composite part as recited in claim 1 or 2, wherein in step S1, the additive manufacturing is by fused deposition modeling, directed energy deposition, or thin-sheet lamination.
10. A continuous fiber reinforced ZrC/SiC composite part product prepared by the preparation method according to any one of claims 1 to 9.
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