CN115650755B - 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 PDFInfo
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Abstract
The application 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, performing 3D printing to obtain a continuous fiber reinforced resin matrix composite material, and performing carbonization and pyrolysis to obtain a continuous fiber block preform; (2) And sequentially depositing pyrolytic carbon and a SiC matrix on the continuous fiber block preform to obtain the continuous fiber toughened silicon carbide ceramic matrix composite material. The continuous fiber reinforced SiC ceramic matrix composite material is prepared by adopting a 3D printing auxiliary chemical vapor deposition technology, the weaving link of a ceramic matrix composite material 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
Technical Field
The application 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 junction components in the fields of aviation, aerospace and brake, and has the advantages of low density, high heat conductivity, friction resistance, thermal shock resistance, low thermal expansion coefficient and the like. However, because the continuous fiber reinforced silicon carbide ceramic matrix composite has the problems of high hardness, difficult processing and the like, a near-shape size forming means is generally adopted to prepare the continuous fiber reinforced silicon carbide ceramic matrix composite member. The weaving of the preform is a main method for forming the near-shape size of the continuous fiber toughened ceramic matrix composite material, and the main weaving method of the continuous fiber preform at present 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 braiding technology is difficult to split due to the constraint of the unidirectional fibers, but braiding equipment is complex, and the braiding period is too long. Meanwhile, in the three-dimensional weaving process, the yarn increasing and decreasing difficulty of the preform is high, the forming period of the preform is further prolonged, and the preparation efficiency of the composite material is affected.
Disclosure of Invention
The application aims to provide a method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite by 3D printing, which solves the problems in the prior art, and the method for preparing the continuous fiber toughened silicon carbide ceramic matrix composite by 3D printing is simple in process, low in cost and wide in application prospect, and the prepared continuous fiber toughened silicon carbide ceramic matrix composite can improve the near-shape size forming efficiency of a preform.
In order to achieve the above object, the present application provides the following solutions:
one of the technical schemes of the application is as follows: a method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite by 3D printing comprises the following steps:
(1) 3D printing is carried out by taking continuous fiber prepreg impregnated with resin (binder) as a printing wire material to obtain a continuous fiber reinforced resin matrix composite material, and then carbonization and pyrolysis are carried out to obtain a continuous fiber block preform;
(2) And sequentially depositing (chemical vapor deposition) pyrolytic carbon and a SiC matrix on the continuous fiber block preform to obtain the continuous fiber toughened silicon carbide ceramic matrix composite material.
Further, in the step (1), the resin includes a phenolic resin, an epoxy resin, or a nylon resin; the continuous fiber prepreg includes carbon fibers (C f ) Or silicon carbide fiber (SiC) f )。
Further, in the step (1), the conditions of the 3D printing 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 more than or equal to 60%.
Further, in the step (1), the carbonization and pyrolysis (heat treatment) temperature is 600-1000 ℃, the heat preservation time is 1h, the flow rate of the protective gas is 600-800 mL/min, and the heating rate and the cooling rate are 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 hours, 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.
Further, the feeding rate of the precursor of the deposited 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 reducing gas flow rate during heating is 1000-3000 mL/min, the shielding gas flow rate is 800-3000 mL/min, the pressure is 1-10 kPa, the cooling rate is 7 ℃/min, and the shielding gas flow rate during cooling is 1000mL/min.
Further, the precursor comprises methyltrichlorosilane; the reducing gas is hydrogen and the shielding gas is argon.
The second technical scheme of the application is as follows: the continuous fiber toughened silicon carbide ceramic matrix composite prepared by the method.
The third technical scheme of the application: the application of the continuous fiber toughened silicon carbide ceramic matrix composite in the preparation of special-shaped components.
The application discloses the following technical effects:
(1) According to the application, the continuous fiber prepreg wire containing the resin is printed into the resin-based composite material by a 3D printer, and then the resin material is converted into pyrolytic carbon by carbonization and pyrolysis, so that the effect of bonding the fiber is achieved, and the continuous fiber block preform is obtained. And then a PyC interface phase and a SiC matrix are deposited on the preform by a chemical vapor deposition technology, so that the continuous fiber reinforced SiC ceramic matrix composite material is obtained, and the weaving links of the ceramic matrix composite material preform are greatly simplified.
(2) The preparation method can overcome the problems that the more complicated the shape and the more complicated the braiding process are for the thermal components with different shapes, thereby greatly improving the manufacturing cost, realizing the rapid molding of the complex component preform of the ceramic matrix composite material and greatly reducing the preparation period and the production cost.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are 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 application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a 3D printing path according to embodiment 1 of the present application, wherein (a) is an odd-layer fiber printing path; (b) print paths for even layers of fibers;
FIG. 2 is a diagram of a process for preparing a continuous fiber reinforced silicon carbide ceramic matrix composite according to example 1 of the present application, wherein (a) is a sample of a continuous fiber reinforced resin matrix composite (cuboid 3D printing), (b) is a continuous fiber reinforced silicon carbide ceramic matrix composite, and (c) is a macroscopic photograph of a continuous fiber reinforced silicon carbide ceramic matrix composite;
FIG. 3 is an SEM image of a process for preparing a continuous fiber-reinforced silicon carbide ceramic-based composite according to example 1 of the present application, wherein (a) is a continuous fiber bulk preform and (b) is a preform having a PyC interface phase (C f @ PyC), (C) is a continuous fiber toughened silicon carbide ceramic matrix composite (C) f @PyC/SiC), (d) is C f The @ PyC fracture morphology and (e) is C f The morphology of the @ PyC/SiC fracture;
FIG. 4 is a schematic diagram of a 3D printing path according to embodiment 2 of the present application;
FIG. 5 is a diagram of a process for preparing a continuous fiber reinforced silicon carbide ceramic matrix composite according to example 2 of the present application, wherein (a) is a sample of a continuous fiber reinforced resin matrix composite (3D printing of a complex profiled member), (b) is a continuous fiber reinforced silicon carbide ceramic matrix composite, and (c) is a macroscopic photograph of a continuous fiber reinforced silicon carbide ceramic matrix composite;
FIG. 6 is a graph showing the bending test results of the continuous fiber-reinforced silicon carbide ceramic matrix composite prepared in example 1 of the present application.
Detailed Description
Various exemplary embodiments of the application will now be described in detail, which should not be considered as limiting the application, but rather as more detailed descriptions of certain aspects, features and embodiments of the application.
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 application. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the application. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, 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 application 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 application. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and materials associated with the documents. 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 application described herein without departing from the scope or spirit of the application. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present application. The specification and examples of the present application are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The purity of Methyltrichlorosilane (MTS) used in the following examples and comparative examples of the present application is greater than 99.90%, the purity of methane gas is greater than 99.90%, and the purity of hydrogen and argon are greater than 99.999%.
Example 1
A method for preparing a continuous fiber toughened silicon carbide ceramic matrix composite by 3D printing comprises the following steps:
(1) Preparation of continuous fiber reinforced resin matrix composite samples: the three-dimensional modeling software is adopted to complete the model construction of the sample, a 3D printing path (see figure 1) is set, carbon fibers are immersed in molten phenolic resin for 5min, cooling is carried out after the immersion is completed, a printing wire (the volume fraction of the carbon fibers in the printing wire is 60%) is obtained, then 3D printing is carried out by adopting the printing wire, 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 speed is 50mm/s. The diameter of the basic nozzle is 0.4mm, the temperature of the printing platform is 60 ℃, and 60 layers are printed to obtain a continuous fiber reinforced resin matrix composite sample.
(2) Preparation of continuous fiber block preform: fixing a continuous fiber reinforced resin matrix composite sample by using graphite paper, placing the continuous fiber reinforced resin matrix composite sample into a graphite crucible, and then placing the continuous fiber reinforced resin matrix composite sample into a heat treatment furnace for carbonization and pyrolysis, wherein the conditions for controlling the carbonization and pyrolysis are as follows: argon (Ar) is introduced as protective gas (the gas flow is 600 mL/min), the temperature is raised to 700 ℃ at the temperature rising rate of 5 ℃/min, the heat is preserved for 1h, and then the temperature is lowered to the room temperature at the temperature lowering rate of 5 ℃/min, so that the continuous fiber block preform is obtained.
(3) Deposition of pyrolytic carbon (deposition of PyC interfacial phase): placing the continuous fiber block preform in an isothermal chemical vapor deposition furnace to deposit pyrolytic carbon, wherein the pyrolytic carbon deposition conditions are as follows: argon is introduced as shielding gas (the gas flow is 800-2000 mL/min), the deposition pressure is controlled to be 1kPa, the temperature is raised to 1000 ℃ at the heating rate of 5 ℃/min, and then methane gas (CH) is introduced 4 The gas flow rate is 800-2000 mL/min) And (3) depositing pyrolytic carbon for 3 hours, and cooling to room temperature at a cooling rate of 7 ℃/min after the deposition is completed, so as to obtain the preform with the PyC interface phase.
(4) Depositing a SiC matrix: placing the preform with the PyC interface phase in a constant temperature zone in an isothermal chemical vapor deposition furnace to deposit the SiC matrix, wherein the conditions for depositing the SiC matrix are as follows: argon is introduced as shielding gas (the gas flow is 800-3000 mL/min), the pressure in the hearth is controlled to be 1.8kPa, the temperature is raised to 1100 ℃ at the heating rate of 5 ℃/min, and H is introduced 2 As reducing gas (gas flow is 1000-3000 mL/min), then precursor (methyltrichlorosilane, MTS) feeding (speed is 2 g/min) is carried out to deposit SiC matrix, the deposition time is 400H, and after the deposition is finished, the H is stopped to be fed in 2 Changing the gas flow of the shielding gas into 1000mL/min, and cooling to room temperature at the cooling rate of 7 ℃/min to obtain the continuous fiber toughened silicon carbide ceramic matrix composite, wherein the preparation process diagram is shown in figure 2, and the SEM diagram is shown in figure 3.
In fig. 2, (a) is a sample of a continuous fiber reinforced resin matrix composite (cuboid 3D printed), (b) is a continuous fiber toughened silicon carbide ceramic matrix composite, and (c) is a macroscopic photograph of a continuous fiber toughened silicon carbide ceramic matrix composite.
In FIG. 3, (a) is a continuous fiber block preform, (b) is a preform (C) having a PyC interface phase f @ PyC), (C) is a continuous fiber toughened silicon carbide ceramic matrix composite (C) f @PyC/SiC), (d) is C f The @ PyC fracture morphology and (e) is C f Fracture morphology of the @ PyC/SiC composite material.
As can be seen from fig. 2, the formation of the fiber preform can be completed by 3D printing means, and the continuous fiber preform is obtained after the heat treatment; as can be seen from fig. 3, after the deposition of the PyC interface phase and the SiC matrix, the PyC phase and the SiC phase completely cover the surface of the carbon fiber, and the interface bonding is good, so that 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 continuous fiber reinforced resin matrix composite samples: the three-dimensional modeling software is adopted to complete the model construction of the sample, a 3D printing path is set (see fig. 4), silicon carbide fibers are immersed in molten epoxy resin for 5min, cooling is carried out after the immersion is completed, a printing wire (the volume fraction of the silicon carbide fibers in the printing wire is 70%), then 3D printing is carried out by adopting the printing wire (the printing wire: resin binder=19:1), 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 speed is 80mm/s. The diameter of the basic nozzle is 0.4mm, the temperature of the printing platform is 50 ℃, and 90 layers are printed to obtain a continuous fiber reinforced resin matrix composite sample.
(2) Preparation of continuous fiber block preform: fixing a continuous fiber reinforced resin matrix composite sample by using graphite paper, placing the continuous fiber reinforced resin matrix composite sample into a graphite crucible, and then placing the continuous fiber reinforced resin matrix composite sample into a heat treatment furnace for carbonization and pyrolysis, wherein the conditions for controlling the carbonization and pyrolysis are as follows: argon (Ar) is introduced as shielding gas (the gas flow is 800 mL/min), the temperature is raised to 1000 ℃ at the temperature rising rate of 5 ℃/min, the heat is preserved for 1h, and then the temperature is lowered to the room temperature at the temperature lowering rate of 5 ℃/min, so that the continuous fiber block preform is obtained.
(3) Deposition of pyrolytic carbon (deposition of PyC interfacial phase): placing the continuous fiber block preform in an isothermal chemical vapor deposition furnace to deposit pyrolytic carbon, wherein the pyrolytic carbon deposition conditions are as follows: argon is introduced as shielding gas (the gas flow is 800-2000 mL/min), the deposition pressure is controlled to be 2kPa, the temperature is raised to 1000 ℃ at the heating rate of 5 ℃/min, and then methane gas (CH) is introduced 4 The gas flow is 800-2000 mL/min), the deposition time is 3h, and after the deposition is completed, the temperature is reduced to room temperature at the cooling rate of 7 ℃/min, and the preform with the PyC interface phase is obtained.
(4) Depositing a SiC matrix: placing the preform with the PyC interface phase in a constant temperature zone in an isothermal chemical vapor deposition furnace to deposit the SiC matrix, wherein the conditions for depositing the SiC matrix are as follows: argon is introduced as shielding gas (the gas flow is 800-3000 mL/min), the pressure in the hearth is controlled to be 1kPa, the temperature is raised to 1100 ℃ at the heating rate of 5 ℃/min, and H is introduced 2 As a reducing gas (gas flow rate is 1000-3000 mL/min), and then a precursor (methyl trichloro)Silane, MTS) feed (rate 1 g/min) deposition of SiC substrate for 300H, stopping H feed after deposition 2 Changing the gas flow of the shielding gas into 1000mL/min, and cooling to room temperature at the cooling rate of 7 ℃/min to obtain the continuous fiber toughened silicon carbide ceramic matrix composite, wherein the preparation process diagram is shown in figure 5.
In fig. 5, (a) is a continuous fiber reinforced resin matrix composite sample (3D printing of a complex profiled member), (b) is a continuous fiber toughened silicon carbide ceramic matrix composite, and (c) is a macroscopic photograph of the continuous fiber toughened silicon carbide ceramic matrix composite.
As can be seen from fig. 5, the formation of the fiber preform can be completed by 3D printing means, and a continuous fiber preform (complex shaped 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 continuous fiber reinforced resin matrix composite samples: the three-dimensional modeling software is adopted to complete the model construction of the sample, a 3D printing path (as shown in fig. 4) is set, silicon carbide fibers (the fiber volume fraction is 60%) are immersed in molten nylon resin for 5min, cooling is carried out after the immersion is completed, a printing wire (the volume fraction of the silicon carbide fibers in the printing wire is 70%) is obtained, then 3D printing is carried out by adopting the printing wire (the printing wire: resin binder=19:1), 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. The diameter of the basic nozzle is 0.4mm, the temperature of the printing platform is 40 ℃, and 90 layers are printed to obtain a continuous fiber reinforced resin matrix composite sample.
(2) Preparation of continuous fiber block preform: fixing a continuous fiber reinforced resin matrix composite sample by using graphite paper, placing the continuous fiber reinforced resin matrix composite sample into a graphite crucible, and then placing the continuous fiber reinforced resin matrix composite sample into a heat treatment furnace for carbonization and pyrolysis, wherein the conditions for controlling the carbonization and pyrolysis are as follows: argon (Ar) is introduced as protective gas (the gas flow is 600 mL/min), the temperature is raised to 800 ℃ at the temperature raising rate of 5 ℃/min, the heat is preserved for 1h, and then the temperature is lowered to room temperature at the temperature lowering rate of 5 ℃/min, so that the continuous fiber block preform is obtained.
(3) Deposition of pyrolytic carbon (deposition of PyC interfacial phase): placing the continuous fiber block preform in an isothermal chemical vapor deposition furnace to deposit pyrolytic carbon, wherein the pyrolytic carbon deposition conditions are as follows: argon is introduced as shielding gas (the gas flow is 800-2000 mL/min), the deposition pressure is controlled to be 2kPa, the temperature is raised to 1100 ℃ at the heating rate of 5 ℃/min, and then methane gas (CH) is introduced 4 The gas flow is 800-2000 mL/min), the deposition time is 3h, and after the deposition is completed, the temperature is reduced to room temperature at the cooling rate of 7 ℃/min, and the preform with the PyC interface phase is obtained.
(4) Depositing a SiC matrix: placing the preform with the PyC interface phase in a constant temperature zone in an isothermal chemical vapor deposition furnace to deposit the SiC matrix, wherein the conditions for depositing the SiC matrix are as follows: argon is introduced as shielding gas (the gas flow is 800-3000 mL/min), the pressure in the hearth is controlled to be 3kPa, the temperature is raised to 1200 ℃ at the heating rate of 5 ℃/min, and H is introduced 2 As reducing gas (gas flow is 1000-3000 mL/min), then precursor (methyltrichlorosilane, MTS) feeding (speed is 3 g/min) is carried out to deposit SiC matrix, the deposition time is 200H, and after the deposition is completed, the H is stopped to be fed in 2 Changing the gas flow of the shielding gas into 1000mL/min, and cooling to room temperature at the cooling rate of 7 ℃/min to obtain the continuous fiber toughened silicon carbide ceramic matrix composite.
Example 4
The difference from example 1 is that the temperature of the carbonization/pyrolysis in step (2) is 600 ℃.
Example 5
The difference from example 1 is that the temperature for depositing pyrolytic carbon in step (3) is 1200 ℃, the deposition pressure is 3kPa, and the deposition time is 10 hours.
Example 6
The difference from example 1 is that the temperature at which the SiC substrate is deposited in step (3) is 900 ℃.
Example 7
The difference from example 1 is that the temperature at which the SiC matrix is deposited in step (3) is 1300 ℃, the pressure in the furnace is 10kPa, and the precursor feed rate is 4g/min.
Effect example 1
The bending performance of the continuous fiber reinforced silicon carbide ceramic matrix composite material prepared by the method is tested, and the bending resistance of the continuous fiber reinforced silicon carbide ceramic matrix composite material reaches 180+/-10 MPa. The stress-strain spectrum is shown in FIG. 6.
The above embodiments are only illustrative of the preferred embodiments of the present application and are not intended to limit the scope of the present application, and various modifications and improvements made by those skilled in the art to the technical solutions of the present application should fall within the protection scope defined by the claims of the present application without departing from the design spirit of the present application.
Claims (5)
1. The method for preparing the continuous fiber toughened silicon carbide ceramic matrix composite by 3D printing is characterized by comprising the following steps of:
(1) Preparation of continuous fiber reinforced resin matrix composite samples: 3D printing paths are set, carbon fibers are immersed in molten phenolic resin for 5min, and cooled after the immersion is finished, so that printing wires are obtained, and the volume fraction of the carbon fibers in the printing wires is 60%; then 3D printing is carried out by adopting the printing wire, the ratio of the printing wire to the resin binder is 19:1, the printing temperature of the printing wire is 265 ℃, and the printing speed is 10mm/s; the resin binder is nylon 66, the printing temperature of the resin binder is 250 ℃, and the speed is 50mm/s; the diameter of the basic nozzle is 0.4mm, the temperature of the printing platform is 60 ℃, and 60 layers are printed to obtain a continuous fiber reinforced resin matrix composite sample;
(2) Preparation of continuous fiber block preform: fixing a continuous fiber reinforced resin matrix composite 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 pyrolysis, wherein the conditions for carbonization and pyrolysis are as follows: argon is introduced as shielding gas, the temperature is raised to 700 ℃ at a heating rate of 5 ℃/min, the temperature is kept for 1h, and then the temperature is lowered to room temperature at a cooling rate of 5 ℃/min, so that a continuous fiber block-shaped preform is obtained;
(3) Depositing pyrolytic carbon: placing the continuous fiber block preform in an isothermal chemical vapor deposition furnace to deposit pyrolytic carbon, wherein the pyrolytic carbon deposition conditions are as follows: argon is introduced as shielding gas, the deposition pressure is controlled to be 1kPa, the temperature is raised to 1000 ℃ at the heating rate of 5 ℃/min, then methane gas is introduced to deposit pyrolytic carbon, the deposition time is 3h, and after the deposition is completed, the temperature is reduced to room temperature at the cooling rate of 7 ℃/min, so as to obtain a preform with a PyC interface phase;
(4) Depositing a SiC matrix: placing the preform with the PyC interface phase in a constant temperature zone in an isothermal chemical vapor deposition furnace to deposit the SiC matrix, wherein the conditions for depositing the SiC matrix are as follows: argon is introduced as shielding gas, the pressure in the hearth is controlled to be 1.8kPa, the temperature is raised to 1100 ℃ at the heating rate of 5 ℃/min, and H is introduced 2 As reducing gas, then precursor feeding is carried out to deposit SiC matrix for 400H, and after the deposition is completed, the H is stopped to be introduced 2 Changing the gas flow of the shielding gas into 1000mL/min, and cooling to room temperature at the cooling rate of 7 ℃/min 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 by 3D printing is characterized by comprising the following steps of:
(1) Preparation of continuous fiber reinforced resin matrix composite samples: 3D printing paths are set, silicon carbide fibers are immersed in molten epoxy resin for 5min, and cooled after the immersion is finished, so that printing wires are obtained, and the volume fraction of the silicon carbide fibers in the printing wires is 70%; then 3D printing is carried out by adopting the printing wire, the ratio of the printing wire to the resin binder is 19:1, the printing temperature of the printing wire is 230 ℃, and the printing speed is 6mm/s; the resin binder is nylon 66, the printing temperature of the resin binder is 240 ℃, and the speed is 80mm/s; the diameter of the basic nozzle is 0.4mm, the temperature of the printing platform is 50 ℃, and 90 layers are printed to obtain a continuous fiber reinforced resin matrix composite sample;
(2) Preparation of continuous fiber block preform: fixing a continuous fiber reinforced resin matrix composite 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 pyrolysis, wherein the conditions for carbonization and pyrolysis are as follows: argon is introduced as shielding gas, the temperature is raised to 1000 ℃ at the heating rate of 5 ℃/min, the heat is preserved for 1h, and then the temperature is reduced to room temperature at the cooling rate of 5 ℃/min, so that a continuous fiber block-shaped preform is obtained;
(3) Depositing pyrolytic carbon: placing the continuous fiber block preform in an isothermal chemical vapor deposition furnace to deposit pyrolytic carbon, wherein the pyrolytic carbon deposition conditions are as follows: argon is introduced as shielding gas, the deposition pressure is controlled to be 2kPa, the temperature is raised to 1000 ℃ at the heating rate of 5 ℃/min, then methane gas is introduced to deposit pyrolytic carbon, the deposition time is 3h, and after the deposition is completed, the temperature is reduced to room temperature at the cooling rate of 7 ℃/min, so as to obtain a preform with a PyC interface phase;
(4) Depositing a SiC matrix: placing the preform with the PyC interface phase in a constant temperature zone in an isothermal chemical vapor deposition furnace to deposit the SiC matrix, wherein the conditions for depositing the SiC matrix are as follows: argon is introduced as shielding gas, the pressure in the hearth is controlled to be 1kPa, the temperature is raised to 1100 ℃ at the heating rate of 5 ℃/min, and H is introduced 2 As reducing gas, then precursor feeding is carried out to deposit SiC matrix, the deposition time is 300H, and after the deposition is finished, the H is stopped being introduced 2 Changing the gas flow of the shielding gas into 1000mL/min, and cooling to room temperature at the cooling rate of 7 ℃/min to obtain the continuous fiber toughened silicon carbide ceramic matrix composite.
3. The method for preparing the continuous fiber toughened silicon carbide ceramic matrix composite by 3D printing is characterized by comprising the following steps of:
(1) Preparation of continuous fiber reinforced resin matrix composite samples: 3D printing paths are set, silicon carbide fibers with the fiber volume fraction of 60% are immersed in molten nylon resin for 5min, and the impregnated silicon carbide fibers are cooled after the immersion is completed, so that printing wires are obtained, and the volume fraction of the silicon carbide fibers in the printing wires is 70%; then 3D printing is carried out by adopting the printing wire, the ratio of the printing wire to the resin binder is 19:1, the printing temperature of the printing wire is 270 ℃, and the printing speed is 9mm/s; the printing temperature of the resin binder is 210 ℃ and the speed is 100mm/s; the diameter of the basic nozzle is 0.4mm, the temperature of the printing platform is 40 ℃, and 90 layers are printed to obtain a continuous fiber reinforced resin matrix composite sample;
(2) Preparation of continuous fiber block preform: fixing a continuous fiber reinforced resin matrix composite 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 pyrolysis, wherein the conditions for carbonization and pyrolysis are as follows: argon is introduced as shielding gas, the temperature is raised to 800 ℃ at the heating rate of 5 ℃/min, the heat is preserved for 1h, and then the temperature is lowered to room temperature at the cooling rate of 5 ℃/min, so that a continuous fiber block-shaped preform is obtained;
(3) Depositing pyrolytic carbon: placing the continuous fiber block preform in an isothermal chemical vapor deposition furnace to deposit pyrolytic carbon, wherein the pyrolytic carbon deposition conditions are as follows: argon is introduced as shielding gas, the deposition pressure is controlled to be 2kPa, the temperature is raised to 1100 ℃ at the heating rate of 5 ℃/min, then methane gas is introduced to deposit pyrolytic carbon for 3 hours, and after the deposition is completed, the temperature is reduced to room temperature at the cooling rate of 7 ℃/min, so as to obtain a preform with a PyC interface phase;
(4) Depositing a SiC matrix: placing the preform with the PyC interface phase in a constant temperature zone in an isothermal chemical vapor deposition furnace to deposit the SiC matrix, wherein the conditions for depositing the SiC matrix are as follows: argon is introduced as protective gas, the pressure in the hearth is controlled to be 3kPa, the temperature is raised to 1200 ℃ at the heating rate of 5 ℃/min, and H is introduced 2 As reducing gas, then precursor feeding is carried out to deposit SiC matrix, the deposition time is 200H, and after the deposition is completed, the H is stopped being introduced 2 Changing the gas flow of the shielding gas into 1000mL/min, and cooling to room temperature at the cooling rate of 7 ℃/min to obtain the continuous fiber toughened silicon carbide ceramic matrix composite.
4. A continuous fiber toughened silicon carbide ceramic matrix composite prepared according to the method of any of claims 1 to 3.
5. Use of the continuous fiber toughened silicon carbide ceramic matrix composite of claim 4 in the preparation of profiled members.
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| CN202211369254.1A CN115650755B (en) | 2022-11-03 | 2022-11-03 | Method for preparing continuous fiber toughened silicon carbide ceramic matrix composite material through 3D printing |
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