CN115650755A - Method for preparing continuous fiber toughened silicon carbide ceramic matrix composite material through 3D printing - Google Patents

Method for preparing continuous fiber toughened silicon carbide ceramic matrix composite material through 3D printing Download PDF

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CN115650755A
CN115650755A CN202211369254.1A CN202211369254A CN115650755A CN 115650755 A CN115650755 A CN 115650755A CN 202211369254 A CN202211369254 A CN 202211369254A CN 115650755 A CN115650755 A CN 115650755A
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continuous fiber
printing
matrix composite
silicon carbide
ceramic matrix
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CN115650755B (en
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冯涛
童明德
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Northwestern Polytechnical University
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Abstract

The invention discloses a method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite material by 3D printing, and belongs to the technical field of 3D printing. The preparation method comprises the following steps: (1) Taking the resin-impregnated continuous fiber prepreg as a printing wire material, performing 3D printing to obtain a continuous fiber reinforced resin matrix composite material, and then performing carbonization cracking to obtain a continuous fiber blocky prefabricated body; (2) And sequentially depositing pyrolytic carbon and a SiC matrix on the continuous fiber massive preform to obtain the continuous fiber toughened silicon carbide ceramic matrix composite. According to the invention, the continuous fiber reinforced SiC ceramic matrix composite is prepared by adopting a 3D printing assisted chemical vapor deposition technology, the weaving link of a ceramic matrix composite preform is greatly simplified, and the prepared material has the advantages of phase stability, high temperature resistance, high strength, oxidation resistance and the like, and has a huge application prospect in the field of aerospace equipment and brake braking.

Description

Method for preparing continuous fiber toughened silicon carbide ceramic matrix composite material through 3D printing
Technical Field
The invention relates to the technical field of 3D printing, in particular to a method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite material by 3D printing.
Background
The continuous fiber reinforced silicon carbide ceramic matrix composite is one of the most potential materials for preparing thermal structural members in the fields of aviation, aerospace and brake, and has a series of advantages of low density, high thermal conductivity, friction resistance, thermal shock resistance, low thermal expansion coefficient and the like. However, because of the problems of large hardness, difficult processing and the like of the continuous fiber reinforced silicon carbide ceramic matrix composite material, the continuous fiber reinforced silicon carbide ceramic matrix composite material member is generally prepared by adopting a near-shape size forming method. The weaving of the preform is a main method for forming the approximate dimension of the continuous fiber toughened ceramic matrix composite, and the current main weaving method of the continuous fiber preform comprises fiber cloth lamination and three-dimensional weaving technology; the fiber cloth lamination technology is simple to operate, but continuous fiber cloth needs to be prepared in advance; the fiber preform prepared by the three-dimensional weaving technology is not easy to be subjected to interlayer disintegration due to the constraint of all-directional fibers, but weaving equipment is complex and the weaving period is too long. Meanwhile, in the three-dimensional weaving process, the yarn increasing and decreasing difficulty of the prefabricated body is high, the forming period of the prefabricated body is further prolonged, and the preparation efficiency of the composite material is influenced.
Disclosure of Invention
The invention aims to provide a method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite material by 3D printing, which aims to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following scheme:
one of the technical schemes of the invention is as follows: a method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite material through 3D printing comprises the following steps:
(1) The method comprises the steps of completing model construction of a sample piece by adopting three-dimensional modeling software, setting a 3D printing path, carrying out 3D printing by taking a continuous fiber prepreg impregnated with resin (binder) as a printing wire material to obtain a continuous fiber reinforced resin matrix composite material, and then carrying out carbonization cracking to obtain a continuous fiber block-shaped prefabricated body;
(2) And sequentially depositing (chemical vapor deposition) pyrolytic carbon and a SiC matrix on the continuous fiber blocky preform to obtain the continuous fiber toughened silicon carbide ceramic matrix composite.
Further, in the step (1), the resin comprises phenolic resin, epoxy resin or nylon resin; the continuous fiber prepreg includes carbon fibers (C) f ) Or silicon carbide fibers (SiC) f )。
Further, in step (1), the 3D printing conditions are: the printing temperature of the resin binder (nylon 66) is 100-250 ℃, and the printing speed is 30-80 cm/s; the printing temperature of the printing wire is 150-300 ℃, and the printing speed is 1-10 cm/s.
Further, in the step (1), the volume fraction of the continuous fiber prepreg in the printing wire is not less than 60%.
Further, in the step (1), the temperature of the carbonization cracking (heat treatment) is 600-1000 ℃, the heat preservation time is 1h, the flow of the protective gas is 600-800 mL/min, and the heating rate and the cooling rate are both 5 ℃/min.
Further, in the step (2), the temperature of the deposited pyrolytic carbon is 900-1200 ℃, the pressure is 1-3 kPa, the deposition time is 3-10 h, the flow rates of the protective gas and methane are 800-2000 mL/min, the heating rate is 5 ℃/min, and the cooling rate is 7 ℃/min.
Furthermore, the feeding rate of the deposition SiC matrix precursor is 1-4 g/min, the heating rate is 5 ℃/min, the deposition temperature is 900-1300 ℃, the deposition time is 200-400 h, the flow rate of reducing gas during heating is 1000-3000 mL/min, the flow rate of protective gas is 800-3000 mL/min, the pressure is 1-10 kPa, the cooling rate is 7 ℃/min, and the flow rate of protective gas during cooling is 1000mL/min.
Further, the precursor comprises methyltrichlorosilane; the reducing gas is hydrogen, and the protective gas is argon.
The second technical scheme of the invention is as follows: a continuous fiber toughened silicon carbide ceramic matrix composite material prepared by the method.
The third technical scheme of the invention is as follows: an application of the continuous fiber toughened silicon carbide ceramic matrix composite material in preparation of a special-shaped component.
The invention discloses the following technical effects:
(1) According to the invention, a continuous fiber prepreg wire containing resin is printed into a resin-based composite material by a 3D printer, and then the resin material is converted into pyrolytic carbon by carbonization and cracking so as to play a role in bonding fibers and obtain a continuous fiber block-shaped preform. And then depositing a PyC interface phase and a SiC matrix on the preform by a chemical vapor deposition technology, thereby obtaining the continuous fiber reinforced SiC ceramic matrix composite and greatly simplifying the weaving link of the ceramic matrix composite preform.
(2) The preparation method can solve the problem that the more complex the shape of the hot component with different shapes is, the more complex the weaving process is, so that the manufacturing cost is greatly increased, can realize the rapid forming of the ceramic matrix composite material complex component prefabricated body, and greatly reduces the preparation period and the production cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a schematic diagram of a 3D printing path according to embodiment 1 of the present invention, wherein (a) is an odd-numbered layer fiber printing path; (b) an even number of layers of fiber print paths;
FIG. 2 is a process diagram of the preparation of the continuous fiber-toughened silicon carbide ceramic matrix composite according to embodiment 1 of the present invention, in which (a) is a continuous fiber-reinforced resin matrix composite sample (rectangular solid 3D printed), (b) is a continuous fiber-toughened silicon carbide ceramic matrix composite, and (c) is a macro photo of the continuous fiber-toughened silicon carbide ceramic matrix composite;
FIG. 3 is an SEM photograph of a continuous fiber toughened silicon carbide ceramic matrix composite prepared according to example 1 of the present invention, wherein (a) is a continuous fiber bulk preform and (b) is a preform with PyC interface phase (C) f @ PyC) and C are continuous fiber toughened silicon carbide ceramic matrix composite material (C) f @ PyC/SiC), (d) is C f The fracture morphology of @ PyC, (e) is C f The fracture morphology of @ PyC/SiC;
FIG. 4 is a schematic diagram of a 3D printing path according to embodiment 2 of the present invention;
FIG. 5 is a process diagram of the preparation of the continuous fiber-toughened silicon carbide ceramic-based composite material in example 2 of the present invention, wherein (a) is a continuous fiber-reinforced resin-based composite material sample (3D printing of a complex profile member), (b) is a continuous fiber-toughened silicon carbide ceramic-based composite material, and (c) is a macro photo of the continuous fiber-toughened silicon carbide ceramic-based composite material;
FIG. 6 is a graph showing the results of a bending test of the continuous fiber toughened silicon carbide ceramic matrix composite prepared in example 1 of the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in the present disclosure, it is understood that each intervening value, to the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated herein by reference to disclose and describe the methods and materials in connection with which the documents are cited. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The following examples and comparative examples of the present invention employed Methyltrichlorosilane (MTS) having a purity of greater than 99.90%, methane gas having a purity of greater than 99.90%, and hydrogen and argon having a purity of greater than 99.999%.
Example 1
A method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite material through 3D printing comprises the following steps:
(1) Preparation of a continuous fiber reinforced resin matrix composite sample: the method comprises the steps of completing model construction of a sample by adopting three-dimensional modeling software, setting a 3D printing path (shown in figure 1), soaking carbon fibers in molten phenolic resin for 5min, cooling after the soaking is completed to obtain a printing wire (the volume fraction of the carbon fibers in the printing wire is 60%), and then performing 3D printing by adopting the printing wire, wherein the printing temperature of the printing wire (the printing wire: resin binder =19 1) is 265 ℃, the printing speed is 10mm/s, the printing temperature of the resin binder (nylon 66) is 250 ℃, and the printing speed is 50mm/s. And (3) printing 60 layers at the temperature of 60 ℃ with the diameter of the basic nozzle being 0.4mm and the temperature of the printing platform to obtain the continuous fiber reinforced resin matrix composite sample.
(2) Preparing a continuous fiber block preform: fixing a continuous fiber reinforced resin matrix composite material sample by using graphite paper, placing the sample into a graphite crucible, and then placing the sample into a heat treatment furnace for carbonization and cracking, wherein the carbonization and cracking conditions are controlled as follows: introducing argon (Ar) as protective gas (the gas flow is 600 mL/min), heating to 700 ℃ at the heating rate of 5 ℃/min, preserving heat for 1h, and then cooling to room temperature at the cooling rate of 5 ℃/min to obtain the continuous fiber block preform.
(3) Pyrolytic carbon deposition (deposition of PyC interphase): putting the continuous fiber blocky preform into an isothermal chemical vapor deposition furnace to deposit pyrolytic carbon, wherein the conditions for depositing the pyrolytic carbon are as follows: introducing argon as protective gas (gas flow is 800-2000 mL/min), controlling deposition pressure to be 1kPa, heating to 1000 ℃ at a heating rate of 5 ℃/min, and then introducing methane gas (CH) 4 Gas flow of 800-2000 mL/min) is deposited for 3h, and after the deposition is finished, the temperature is reduced to room temperature at the cooling rate of 7 ℃/min, so that a preform with a PyC interface phase is obtained.
(4) Depositing a SiC matrix: placing the preform with the PyC interface phase in a constant-temperature area in an isothermal chemical vapor deposition furnace to deposit a SiC matrix, wherein the conditions for depositing the SiC matrix are as follows: introducing argon as protective gas (gas flow is 800-3000 mL/min), controlling the pressure in the hearth to be 1.8kPa, heating to 1100 ℃ at the heating rate of 5 ℃/min, and introducing H 2 Taking the SiC as reducing gas (the gas flow is 1000-3000 mL/min), then carrying out precursor (methyl trichlorosilane, MTS) feeding (the speed is 2 g/min) to deposit the SiC matrix, the deposition time is 400H, and stopping introducing H after the deposition is finished 2 Changing the gas flow of the protective gas to 1000mL/min, and cooling to room temperature at a cooling rate of 7 ℃/min to obtain the continuous fiber toughened silicon carbide ceramic-based composite material, wherein a preparation process diagram is shown in figure 2, and an SEM diagram is shown in figure 3.
In fig. 2, (a) is a continuous fiber reinforced resin matrix composite sample (rectangular 3D printed), (b) is a continuous fiber toughened silicon carbide ceramic matrix composite, and (c) is a macro photograph of the continuous fiber toughened silicon carbide ceramic matrix composite.
In FIG. 3, (a) is a continuous fiber blockA preform having a PyC interface phase (C) f @ PyC) and C are continuous fiber toughened silicon carbide ceramic matrix composite material (C) f @ PyC/SiC), (d) is C f The fracture morphology of @ PyC, (e) is C f The fracture morphology of the @ PyC/SiC composite material.
As can be seen from fig. 2, the molding of the fiber preform can be completed by 3D printing means, and a continuous fiber preform is obtained after heat treatment; as can be seen from FIG. 3, after the deposition of the PyC interface phase and the SiC matrix, the PyC and SiC phases are completely covered on the surface of the carbon fiber, the interface bonding is good, and no obvious shedding phenomenon occurs.
Example 2
A method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite by 3D printing comprises the following steps:
(1) Preparation of a continuous fiber reinforced resin matrix composite sample: the method comprises the steps of completing model construction of a sample by adopting three-dimensional modeling software, setting a 3D printing path (shown in figure 4), soaking silicon carbide fibers in molten epoxy resin for 5min, cooling after the soaking is completed to obtain a printing wire (the volume fraction of the silicon carbide fibers in the printing wire is 70%), and then performing 3D printing (the printing wire: resin binder =19: 1) by adopting the printing wire, wherein the printing temperature of the printing wire is 230 ℃, the printing speed is 6mm/s, the printing temperature of the resin binder (nylon 66) is 240 ℃ and the printing speed is 80mm/s. And (3) printing 90 layers at the temperature of 50 ℃ with the diameter of the basic nozzle being 0.4mm and the temperature of the printing platform to obtain the continuous fiber reinforced resin matrix composite sample.
(2) Preparing a continuous fiber block preform: fixing a continuous fiber reinforced resin matrix composite material sample by using graphite paper, placing the sample into a graphite crucible, and then placing the sample into a heat treatment furnace for carbonization and cracking, wherein the carbonization and cracking conditions are controlled as follows: introducing argon (Ar) as protective gas (the gas flow is 800 mL/min), heating to 1000 ℃ at the heating rate of 5 ℃/min, preserving heat for 1h, and then cooling to room temperature at the cooling rate of 5 ℃/min to obtain the continuous fiber block preform.
(3) Pyrolytic carbon deposition (deposition of PyC interphase): putting the continuous fiber block-shaped prefabricated body into an isothermal chemical vapor deposition furnace for depositionDepositing pyrolytic carbon under the following conditions: introducing argon as protective gas (gas flow is 800-2000 mL/min), controlling deposition pressure to be 2kPa, heating to 1000 ℃ at a heating rate of 5 ℃/min, and then introducing methane gas (CH) 4 Gas flow of 800-2000 mL/min) is deposited for 3h, and after the deposition is finished, the temperature is reduced to room temperature at the cooling rate of 7 ℃/min, so that a preform with a PyC interface phase is obtained.
(4) Depositing a SiC matrix: placing the preform with the PyC interface phase in a constant-temperature area in an isothermal chemical vapor deposition furnace to deposit a SiC matrix, wherein the conditions for depositing the SiC matrix are as follows: introducing argon as protective gas (gas flow is 800-3000 mL/min), controlling the pressure in the hearth to be 1kPa, heating to 1100 ℃ at the heating rate of 5 ℃/min, and introducing H 2 Taking the precursor (methyl trichlorosilane, MTS) as reducing gas (the gas flow is 1000-3000 mL/min), then feeding the precursor (methyl trichlorosilane, MTS) (the speed is 1 g/min) to deposit the SiC matrix, the deposition time is 300H, and stopping introducing H after the deposition is finished 2 Changing the gas flow of the protective gas to 1000mL/min, and cooling to room temperature at a cooling rate of 7 ℃/min to obtain the continuous fiber toughened silicon carbide ceramic-based composite material, wherein a preparation process chart is shown in FIG. 5.
In fig. 5, (a) is a continuous fiber reinforced resin matrix composite sample (3D printing of a complex irregular member), (b) is a continuous fiber toughened silicon carbide ceramic matrix composite, and (c) is a macro photograph of the continuous fiber toughened silicon carbide ceramic matrix composite.
As can be seen from fig. 5, the shaping of the fiber preform can be accomplished by 3D printing means, and a continuous fiber preform (complex profile member) is obtained after heat treatment.
Example 3
A method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite by 3D printing comprises the following steps:
(1) Preparation of a continuous fiber reinforced resin matrix composite sample: the method comprises the steps of completing model construction of a sample by adopting three-dimensional modeling software, setting a 3D printing path (as shown in figure 4), soaking silicon carbide fibers (the volume fraction of fibers is 60%) in molten nylon resin for 5min, cooling after the soaking is completed to obtain a printing wire (the volume fraction of the silicon carbide fibers in the printing wire is 70%), and then performing 3D printing (the printing wire: resin binder = 19) by adopting the printing wire, wherein the printing temperature of the printing wire is 270 ℃, the printing speed is 9mm/s, the printing temperature of the resin binder is 210 ℃ and the printing speed is 100mm/s. And (3) printing 90 layers at the temperature of 40 ℃ with the diameter of the basic nozzle being 0.4mm and the temperature of the printing platform to obtain the continuous fiber reinforced resin matrix composite sample.
(2) Preparing a continuous fiber block preform: fixing a continuous fiber reinforced resin matrix composite material sample by using graphite paper, placing the sample into a graphite crucible, and then placing the sample into a heat treatment furnace for carbonization and cracking, wherein the carbonization and cracking conditions are controlled as follows: introducing argon (Ar) as protective gas (the gas flow is 600 mL/min), heating to 800 ℃ at the heating rate of 5 ℃/min, preserving heat for 1h, and then cooling to room temperature at the cooling rate of 5 ℃/min to obtain the continuous fiber block preform.
(3) Pyrolytic carbon deposition (deposition of PyC interphase): putting the continuous fiber blocky preform into an isothermal chemical vapor deposition furnace to deposit pyrolytic carbon, wherein the conditions for depositing the pyrolytic carbon are as follows: introducing argon as protective gas (gas flow is 800-2000 mL/min), controlling deposition pressure to be 2kPa, heating to 1100 ℃ at a heating rate of 5 ℃/min, and then introducing methane gas (CH) 4 Gas flow of 800-2000 mL/min) is deposited for 3h, and after the deposition is finished, the temperature is reduced to room temperature at the cooling rate of 7 ℃/min, so that a preform with a PyC interface phase is obtained.
(4) Deposition of a SiC matrix: placing the preform with the PyC interface phase in a constant-temperature area in an isothermal chemical vapor deposition furnace to deposit a SiC matrix, wherein the conditions for depositing the SiC matrix are as follows: introducing argon as protective gas (gas flow is 800-3000 mL/min), controlling the pressure in the hearth to be 3kPa, heating to 1200 ℃ at the heating rate of 5 ℃/min, and introducing H 2 Taking the precursor (methyl trichlorosilane, MTS) as reducing gas (the gas flow is 1000-3000 mL/min), then feeding the precursor (methyl trichlorosilane, MTS) (the speed is 3 g/min) to deposit the SiC matrix, the deposition time is 200H, and stopping introducing H after the deposition is finished 2 Changing the gas flow of the protective gas to 1000mL/min, and reducing the temperature at a rate of 7 ℃/minAnd (5) heating to room temperature to obtain the continuous fiber toughened silicon carbide ceramic matrix composite.
Example 4
The difference from example 1 is that the temperature for the pyrolysis in step (2) is 600 ℃.
Example 5
The difference from example 1 is that the temperature for depositing the pyrolytic carbon in step (3) is 1200 deg.C, the deposition pressure is 3kPa, and the deposition time is 10 hours.
Example 6
The difference from example 1 is that the temperature for depositing the SiC matrix in step (3) is 900 ℃.
Example 7
The difference from example 1 is that the SiC substrate deposited in step (3) was at a temperature of 1300 ℃, a pressure in the furnace was 10kPa, and a precursor feed rate was 4g/min.
Effect example 1
The bending property of the continuous fiber reinforced silicon carbide ceramic matrix composite material prepared by the method is tested, and the bending property of the composite material reaches 180 +/-10 MPa. The stress-strain spectrum is shown in FIG. 6.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (10)

1. A method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite material through 3D printing is characterized by comprising the following steps:
(1) Taking the resin-impregnated continuous fiber prepreg as a printing wire material, performing 3D printing to obtain a continuous fiber reinforced resin matrix composite material, and then performing carbonization cracking to obtain a continuous fiber blocky prefabricated body;
(2) And sequentially depositing pyrolytic carbon and a SiC matrix on the continuous fiber massive preform to obtain the continuous fiber toughened silicon carbide ceramic matrix composite.
2. The method for preparing the continuous fiber toughened silicon carbide ceramic matrix composite material by 3D printing according to claim 1, wherein in step (1), the resin comprises phenolic resin, epoxy resin or nylon resin; the continuous fiber prepreg includes carbon fibers or silicon carbide fibers.
3. The method for preparing the continuous fiber toughened silicon carbide ceramic matrix composite material by 3D printing according to claim 1, wherein in the step (1), the 3D printing conditions are as follows: the printing temperature of the resin binder is 100-250 ℃, and the printing speed is 30-80 cm/s; the printing temperature of the printing wire is 150-300 ℃, and the printing speed is 1-10 cm/s.
4. The method for preparing the continuous fiber toughened silicon carbide ceramic matrix composite material by 3D printing according to claim 1, wherein in the step (1), the volume fraction of the continuous fiber prepreg in the printing wire is not less than 60%.
5. The method for preparing the continuous fiber toughened silicon carbide ceramic matrix composite material by 3D printing according to claim 1, wherein in the step (1), the temperature of carbonization cracking is 600-1000 ℃, the holding time is 1h, the flow of protective gas is 600-800 mL/min, and the heating rate and the cooling rate are both 5 ℃/min.
6. The method for preparing the continuous fiber toughened silicon carbide ceramic matrix composite material by 3D printing according to claim 1, wherein in the step (2), the temperature of the deposited pyrolytic carbon is 900-1200 ℃, the pressure is 1-3 kPa, the deposition time is 3-10 h, the flow rates of the protective gas and methane are 800-2000 mL/min, the heating rate is 5 ℃/min, and the cooling rate is 7 ℃/min.
7. The method for preparing the continuous fiber toughened silicon carbide ceramic matrix composite material by 3D printing according to claim 1, wherein in the step (2), the feeding rate of the precursor for depositing the SiC matrix is 1-4 g/min, the heating rate is 5 ℃/min, the deposition temperature is 900-1300 ℃, the deposition time is 200-400 h, the flow rate of the reducing gas during heating is 1000-3000 mL/min, the flow rate of the protective gas during heating is 800-3000 mL/min, the pressure is 1-10 kPa, the cooling rate is 7 ℃/min, and the flow rate of the protective gas during cooling is 1000mL/min.
8. The method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite according to claim 7, wherein the precursor comprises methyltrichlorosilane; the reducing gas is hydrogen, and the protective gas is argon.
9. A continuous fiber toughened silicon carbide ceramic matrix composite prepared according to the method of any one of claims 1 to 8.
10. Use of the continuous fiber toughened silicon carbide ceramic matrix composite according to claim 9 in the preparation of a profiled element.
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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106278335A (en) * 2016-08-05 2017-01-04 西安交通大学 A kind of manufacture method of fiber alignment toughening ceramic based composites turbo blade
CN106866164A (en) * 2017-02-27 2017-06-20 西安交通大学 A kind of ceramic composite manufacturing process based on fiber reinforced ceramic precursor 3D printing technique
CN110171976A (en) * 2019-05-27 2019-08-27 华中科技大学 The preparation method and product of SiC base ceramic part based on increasing material manufacturing
US20190330119A1 (en) * 2017-04-13 2019-10-31 Huazhong University Of Science And Technology Method of preparing carbon fiber reinforced carbon-silicon carbide composite part
CN110862264A (en) * 2019-09-11 2020-03-06 中国科学院金属研究所 Continuous silicon carbide fiber reinforced silicon carbide ceramic matrix composite material and preparation method and application thereof
CN111662091A (en) * 2020-06-15 2020-09-15 中国科学院上海硅酸盐研究所 Short carbon fiber reinforced Csf/SiC ceramic matrix composite material and preparation method thereof
CN113787710A (en) * 2021-09-08 2021-12-14 西安交通大学 3D printing system and method for continuous fiber reinforced thermosetting resin composite material
CN114230347A (en) * 2021-12-24 2022-03-25 华中科技大学 Preparation method and product of continuous fiber reinforced ZrC/SiC composite part
CN115073196A (en) * 2022-07-15 2022-09-20 北京理工大学 Additive manufacturing and forming method for continuous fiber reinforced ceramic matrix composite material

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106278335A (en) * 2016-08-05 2017-01-04 西安交通大学 A kind of manufacture method of fiber alignment toughening ceramic based composites turbo blade
CN106866164A (en) * 2017-02-27 2017-06-20 西安交通大学 A kind of ceramic composite manufacturing process based on fiber reinforced ceramic precursor 3D printing technique
US20190330119A1 (en) * 2017-04-13 2019-10-31 Huazhong University Of Science And Technology Method of preparing carbon fiber reinforced carbon-silicon carbide composite part
CN110171976A (en) * 2019-05-27 2019-08-27 华中科技大学 The preparation method and product of SiC base ceramic part based on increasing material manufacturing
CN110862264A (en) * 2019-09-11 2020-03-06 中国科学院金属研究所 Continuous silicon carbide fiber reinforced silicon carbide ceramic matrix composite material and preparation method and application thereof
CN111662091A (en) * 2020-06-15 2020-09-15 中国科学院上海硅酸盐研究所 Short carbon fiber reinforced Csf/SiC ceramic matrix composite material and preparation method thereof
CN113787710A (en) * 2021-09-08 2021-12-14 西安交通大学 3D printing system and method for continuous fiber reinforced thermosetting resin composite material
CN114230347A (en) * 2021-12-24 2022-03-25 华中科技大学 Preparation method and product of continuous fiber reinforced ZrC/SiC composite part
CN115073196A (en) * 2022-07-15 2022-09-20 北京理工大学 Additive manufacturing and forming method for continuous fiber reinforced ceramic matrix composite material

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