Device and method for preparing fiber-reinforced SiC ceramic-based composite material based on Joule thermochemical vapor infiltration

Abstract

The invention discloses a device and a method for preparing a fiber-reinforced SiC ceramic-based composite material based on Joule thermochemical vapor infiltration. The device is specifically characterized in that a graphite clamp and a fiber preform are arranged in a reactor, a trichloromethylsilane container, a flowing protective gas introduction device and a tail gas treatment device are respectively communicated with the reactor through gas pipes, and the fiber preform is connected with an external power supply through fibers extending outwards; the preparation method comprises the following steps: putting a fiber fabric preform and a graphite clamp into a reactor, connecting the fiber preform into a circuit, heating the interior of the fiber preform, introducing methyltrichlorosilane and hydrogen into the reactor, turning off a power supply, and cooling a sample to room temperature, thereby completing the preparation. Local high temperature is formed through Joule heat, heating is conducted from the inside to the outside of the preform, SiC is deposited on the fiber preform from inside to outside, so that the material achieves high uniformity, internal pores are reduced, and the density and the deposition rate are improved.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of fiber-reinforced SiC ceramic matrix composite material preparation, in particular to a device and method for preparing fiber-reinforced SiC ceramic matrix composite material based on a chemical vapor deposition method improved according to the principle of Joule heat. BACKGROUND

[0002] The fiber-reinforced SiC ceramic matrix composite material is mainly used in the fields of aerospace, energy, nuclear energy, national defense and military industry, semiconductors and automobiles. The preparation process includes chemical vapor infiltration (CVI), polymer impregnation and pyrolysis (PIP) and melt infiltration (MI) processes. The patent "Method for preparing ceramic matrix composite material through improved PIP process" (application number: CN202510088178.4) prepares the ceramic matrix composite material through polymer impregnation, low-temperature pre-pyrolysis and high-temperature pyrolysis and the like. The patent "Rapidly densified ceramic matrix composite slurry, preparation method and application thereof" (application number: CN202510375025.8) prepares the ceramic matrix composite material by immersing a mixed slurry of polycarbosilane, SiC whisker, calcium fluoride and lanthanum oxide into the composite material. The patent "Nearly fully dense carbon fiber-reinforced ceramic matrix composite material and preparation method thereof" (application number: CN202510526532.7) embeds C f / PyC / silicon carbide matrix in metal powder for reaction melt infiltration to obtain the carbon fiber-reinforced ceramic matrix composite material.

[0003] The obvious shrinkage of the liquid precursor in the PIP method during drying and pyrolysis can damage the fibers of the preform, and the excessively high temperature in the melt infiltration process of the MI method can also cause great damage to the fibers. The CVI process is to direct the gaseous precursor to the fiber braid through diffusion or under the action of a pressure difference, and diffuse into the fiber braid. The gaseous precursor reacts in the pores of the braid under 900-1100 o C to generate a solid product deposited on the pore wall, and the pore wall gradually thickens with the reaction. The method has the advantages of being capable of obtaining a high-purity and high-crystallinity SiC matrix and being suitable for preparing large-size and complex-shaped parts. In the CVI process, the surface pores of the preform need to be kept open to ensure the diffusion of the precursor. However, the conventional chemical vapor infiltration process has the problems of long single deposition time, uneven material deposition, higher porosity in the center of the material than in the outside of the material, low final forming density of the material and high porosity of the material, which can reach 10-15%. In actual CVI process production, it is difficult to realize net-size forming of the ceramic composite material and ensure the consistency of the product. SUMMARY

[0004] The application aims to provide a low porosity fiber reinforced SiC ceramic matrix composite material preparation device and method to solve the problems in the technical background.

[0005] To achieve the above-mentioned purpose, the application provides a device and method for preparing fiber reinforced SiC ceramic matrix composite material based on Joule heat improved chemical vapor deposition, and the core method is to use the principle of Joule heat generation to perform CVI process in different parts of the composite material, set an improved CVI reactor, and realize high densification of the composite material.

[0006] One kind is a device for preparing fiber reinforced SiC ceramic matrix composite material based on Joule heat chemical vapor infiltration The device comprises a flowing protective gas introduction device, a tail gas treatment device, a graphite clamp, a fiber preform, a chloromethylsilane container, a reactor, a gas pipe and a valve; The graphite clamp holds the fiber preform, and the reactor is connected with a plurality of gas pipes, each of which is provided with a corresponding valve.

[0007] The reactor is mainly composed of a quartz tube and metal flanges at both ends of the quartz tube for sealing the quartz tube; the graphite clamp has an upper and lower two-layer structure, and a plurality of circular holes are distributed on the surfaces of the upper and lower clamping pieces, which facilitates the full contact of the gas with the fiber preform; the fiber preform contains a plurality of fibers connected to the electrodes as heat sources.

[0008] The chloromethylsilane container is further provided with a heating jacket, the chloromethylsilane container contains chloromethylsilane and is connected with an air inlet pipe, and the air inlet pipe is provided with an air inlet valve for introducing carrier gas.

[0009] It also includes a power supply, an electrode and a wire, the power supply is connected to the outside of the reactor through the wire, the fiber preform is electrically connected to the two ends of the power supply through the wire, a plurality of fibers are led out from the two ends of the fiber preform, each fiber at each end is connected to the metal flange at the corresponding end, one end of the fiber is connected to the metal flange at the corresponding end, and the other end of the fiber is also connected to the metal flange at the corresponding end, an electrode is arranged on the metal flange at each end of the quartz tube of the reactor, each fiber at each end is connected to the electrode of the metal flange at the corresponding end, and the electrodes of the metal flanges at both ends of the quartz tube of the reactor are electrically connected to the two ends of the power supply through the wire.

[0010] Two, a method for preparing fiber-reinforced SiC ceramic matrix composite by Joule heat chemical vapor infiltration using the device The preparation method comprises the following steps: Based on the rapid formation of high-temperature region by Joule heat, SiC is rapidly deposited inside the fiber preform.

[0011] 1) Place the fiber preform in a confined graphite clamp, and place the graphite clamp in the reactor, with all the valves closed; The step 1) is specifically: Place the fiber preform in a confined graphite clamp, then open the metal flanges on both sides of the quartz tube, and place the graphite clamp holding the fiber preform in the reactor; The fiber preform is one of a one-dimensional fiber bundle of SiC fibers, a two-dimensional fiber woven cloth of SiC fibers, a three-dimensional fiber woven body of SiC fibers, a one-dimensional fiber bundle of C fibers, a two-dimensional fiber woven cloth of C fibers, or a three-dimensional fiber woven body of C fibers. The vacuum pump has good corrosion resistance.

[0012] 2) Connect each fiber at each end to the electrode of the metal flange at the corresponding end, then vacuumize the inside of the reactor, and maintain the vacuum inside the reactor; The step 2) is specifically: Connect each fiber at each end to the electrode of the metal flange at the corresponding end, close the metal flanges on both sides of the quartz tube, and vacuumize the inside of the reactor to below 15 KPa by the vacuum pump through the air pipe or other means, and maintain the vacuum inside the reactor.

[0013] 3) Turn on the power supply, and pass current through the fiber preform by the power supply, while the multiple fiber heat sources in the fiber preform generate Joule heat, so that the temperature of the fiber preform rises; The step 3) is specifically: Turn on the power supply, and pass current through each fiber at each end by the power supply in turn, so that the whole fiber preform is passed through current, while the multiple fiber heat sources in the fiber preform generate Joule heat, so that the temperature of the fiber preform rises. The power supply is a direct current or alternating current power supply with adjustable voltage and current, the voltage adjustment range is 0-36 V, and the current adjustment range is 0-150 A. The flow rate of the trichloromethylsilane is related to the hydrogen gas as the carrier gas, and the flow rate is 1-100 mL / min.

[0014] 4) the trichloromethylsilane container is connected with a gas inlet valve, and hydrogen is used as the carrier gas to bubble into the trichloromethylsilane container through the gas inlet pipe while the heating jacket is started to heat the trichloromethylsilane container to vaporize the liquid, and then the valve between the trichloromethylsilane container and the reactor is opened to make the mixed gas of trichloromethylsilane and hydrogen enter the reactor; the gas generated in the reaction is introduced into the tail gas treatment device; The step 4) is specifically: The gas inlet valve outside the trichloromethylsilane container is opened, hydrogen is used as the carrier gas to bubble into the trichloromethylsilane container through the gas inlet pipe by the bubbling method while the heating jacket is started to heat the trichloromethylsilane container to vaporize the liquid, and then the valve between the trichloromethylsilane container and the reactor is opened to make the mixed gas of trichloromethylsilane and hydrogen enter the reactor; wherein the trichloromethylsilane is used as the deposition gas source. At the same time, the valve between the tail gas treatment device and the reactor is opened, and the HCl gas generated in the reaction is introduced into the tail gas treatment device containing a 5-20wt% NaOH solution, the reaction time is 1-3h, and the reaction temperature is 900-1200℃.

[0015] 5) after the reaction is completed, the power is turned off, the mixed gas of trichloromethylsilane and hydrogen is stopped, a flowing protective gas is introduced, and the composite material is cooled to room temperature in a protective atmosphere; The step 5) is specifically: After the deposition reaction time is completed, the power is turned off, the valve between the trichloromethylsilane container and the reactor is closed, the mixed gas of trichloromethylsilane and hydrogen is stopped, the valve between the flowing protective gas introduction device and the reactor is opened, a flowing protective gas is introduced, the flowing protective gas introduction device is a gas source or other device, the composite material is cooled to room temperature in a protective gas atmosphere, the metal flanges on both sides of the quartz tube are opened, and the composite material is taken out. The protective gas is argon or nitrogen, and the flow rate is 30-250mL / min.

[0016] The application is based on the characteristics of Joule heat principle, and has a fast heating rate, can be heated to 1200 DEG C in 30s-2min, and only needs 10-30min to cool to room temperature, improves the traditional CVI process, designs a Joule heat and CVI combined device for preparing fiber reinforced SiC composite material, and the fabric is gradually heated and deposited from inside to outside, aims to significantly improve the deposition uniformity of the center and the outside of the composite material, improve the density, and reduce the porosity of the composite material. The core innovation point of the application is that the local high temperature area is formed by using Joule heat, the fabric preform is gradually heated from inside to outside, SiC is deposited in the fiber preform first, and then SiC is gradually deposited outward, so that the composite material reaches high uniformity, reduces internal pores, improves density and deposition rate. The technology avoids the problem that the surface is deposited first in the process of traditional chemical vapor infiltration from outside to inside, the channel for gas infiltration into the interior is blocked, and the internal porosity problem is caused. The application provides a new technology for preparing high-density fiber reinforced ceramic matrix composite materials.

[0017] The beneficial effects of the application are: 1. The application is based on the heating principle of Joule heat, a local high temperature is formed by using Joule heat, an improved CVI device is designed, heat is generated in the fiber preform from inside to outside, SiC deposition of the preform occurs from inside to outside, the material reaches high uniformity, SiC is gradually deposited on the outside of the material through heat conduction, the material deposition uniformity is achieved, the internal pores are reduced, and the porosity, density and deposition rate are improved. The technology avoids the internal porosity problem.

[0018] 2. The heating principle of the application is based on Joule heat, and the CVI time can be significantly shortened, and the CVI efficiency can be improved. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 The reaction device for preparing the improved chemical vapor deposition of the fiber reinforced ceramic matrix composite material is a schematic view. Figure 2 The fiber reinforced ceramic matrix composite material of Example 1 is a physical picture. Figure 3 The stress-strain curve of the fiber reinforced ceramic matrix composite material of Example 2 is a stress-strain curve. Figure 4 The cross-sectional morphology of the fiber reinforced ceramic matrix composite material of Example 3 is a cross-sectional morphology. Figure 5 The fiber surface morphology of the fiber preform of Comparative Example 1 is a fiber surface morphology.

[0020] In the figure: 1-Graphite clamp, 2-Fiber preform, 3-Trichloromethylsilane container, 4-Quartz tube, 5-Metal flange, 6-Gas pipe, 7-Valve, 8-Flow protective gas introduction device, 9-Tail gas treatment device, 10-Heating jacket, 11-Electrode, 12-Power supply, 13-Fiber, 14-Wire. Detailed Implementation

[0021] The present invention will be further described below with reference to the accompanying drawings and specific preferred embodiments, but this does not limit the scope of protection of the present invention.

[0022] like Figure 1 As shown, this device includes a flow protective gas inlet device 8, an exhaust gas treatment device 9, a graphite clamp 1, a fiber preform 2, a trichloromethylsilane container 3, a reactor, gas pipes 6, and valves 7. The reactor contains the graphite clamp 1 and the fiber preform 2, with the graphite clamp 1 holding the fiber preform 2. Multiple gas pipes 6 are connected to the outside of the reactor, and each gas pipe 6 is equipped with a corresponding valve 7. The trichloromethylsilane container 3, the flow protective gas inlet device 8, and the exhaust gas treatment device 9 are all connected to the reactor through the gas pipes 6.

[0023] The reactor is mainly composed of a quartz tube 4 and metal flanges 5 at both ends for sealing the quartz tube 4; the graphite clamp 1 has a two-layer structure, and multiple circular holes are distributed on the surface of both layers of the upper and lower clamps, which is conducive to the full contact between the gas and the fiber preform 2. The fiber preform 2 includes multiple fibers 13 and multiple fiber heat sources are present in the fiber preform 2.

[0024] A heating jacket 10 is also provided on the outer periphery of the trichloromethylsilane container 3. The trichloromethylsilane container 3 contains trichloromethylsilane and is connected to an inlet pipe. An inlet valve is provided on the inlet pipe for introducing carrier gas.

[0025] It also includes a power supply 12, electrodes 11, and wires 14. The power supply 12 is electrically connected to the outside of the reactor through the wires 14. Both ends of the fiber preform 2 are electrically connected to the two ends of the power supply 12 through the wires 14. Multiple fibers 13 are led outward from both ends of the fiber preform 2. Each fiber 13 at each end is connected to the metal flange 5 at its corresponding end. The fiber 13 at one end is connected to the metal flange 5 at its corresponding end, and the fiber 13 at the other end is also connected to its corresponding metal flange 5. An electrode 11 is respectively provided on the metal flange 5 at both ends of the reactor quartz tube 4. Each fiber 13 at each end is connected to the electrode 11 at its corresponding end of the metal flange 5. The electrodes 11 at both ends of the reactor quartz tube 4 are electrically connected to the two ends of the power supply 11 through the wires 14.

[0026] Examples of the preparation method using this device are as follows: Example 1 (1) Place about 15 pieces of SiC fiber woven fabric in graphite fixture 1, and then put them into the reactor; (2) Connect the heating fiber 13 to the electrode 11, seal the reactor, evacuate the reactor to 5 kPa, and introduce argon gas to bring the gas pressure in the reactor to atmospheric pressure. (3) Turn on power supply 12, adjust the voltage to 36V, adjust the current to 6A, and heat fiber 13 to 1000℃; (4) Heat trichloromethylsilane to 70°C to produce trichloromethylsilane gas. Turn on the hydrogen gas as a carrier gas to allow the hydrogen and trichloromethylsilane mixture to enter the reactor. The hydrogen flow rate is 10 mL / min. (5) After the reaction has proceeded for 10 minutes, turn off the power supply 12; (6) After turning off power 12, stop the flow of the mixed gas of trichloromethylsilane and hydrogen, and introduce flowing nitrogen at a flow rate of 100 mL / min. Cool to room temperature in a nitrogen environment. (7) After the reactor has cooled to room temperature, open the metal flanges 5 on both sides of the quartz tube 4 and remove the SiC. f / SiC ceramic matrix composites such as Figure 2 As shown.

[0027] Example 2 (1) Place the 3D woven C-fiber preform in the graphite fixture 1 and then put it into the reactor; (2) Connect the heating fiber 13 to the electrode 11, seal the reactor, and evacuate the reactor to 10 kPa; (3) Turn on power supply 12, adjust the voltage to 20V, adjust the current to 10A, and heat the fiber 13 to 1000℃; (4) Heat trichloromethylsilane to 70°C to produce trichloromethylsilane gas. Turn on the hydrogen gas as a carrier gas to allow the hydrogen and trichloromethylsilane mixture to enter the reactor. The hydrogen flow rate is 5 mL / min. (5) Turn off the power supply 12 after the reaction has been going on for 1 hour; (6) After turning off power supply 12, stop the flow of the mixed gas of trichloromethylsilane and hydrogen, and introduce flowing argon gas at a flow rate of 150 mL / min. Cool to room temperature in a nitrogen atmosphere. (7) After the reactor has cooled to room temperature, open the metal flanges 5 on both sides of the quartz tube 4 and remove C. f / SiC ceramic matrix composites; (8) C after Joule heat treatment f The stress-strain curves of the SiC ceramic matrix composite material after multiple impregnation and pyrolysis with polycarbosilane precursors are shown below. Figure 3 As shown, the curve exhibits obvious pseudo-plastic fracture.

[0028] Example 3 (1) Place the 3D braided SiC fiber preform in the graphite fixture 1 and then put it into the reactor; (2) Connect the heating fiber 13 to the electrode 11, seal the reactor, and evacuate the reactor to 10 kPa; (3) Turn on power supply 12, adjust the voltage to 20V, adjust the current to 10A, and heat the fiber 13 to 1000℃; (4) Heat trichloromethylsilane to 70°C to produce trichloromethylsilane gas. Turn on the hydrogen gas as a carrier gas to allow the hydrogen and trichloromethylsilane mixture to enter the reactor. The hydrogen flow rate is 5 mL / min. (5) Turn off the power after the reaction has lasted for 30 minutes. (6) After turning off power supply 12, stop the flow of the mixed gas of trichloromethylsilane and hydrogen, and introduce flowing argon gas at a flow rate of 150 mL / min. Cool to room temperature in a nitrogen atmosphere. (7) After the reactor has cooled to room temperature, open the metal flanges 5 on both sides of the quartz tube 4 and remove the SiC. f / SiC ceramic matrix composites; (8) The obtained SiC f The microstructure of SiC ceramic matrix composites is as follows: Figure 4 As shown, a large amount of SiC matrix can be observed between the fibers. This demonstrates that CVI via Joule heating can significantly improve the deposition efficiency of SiC.

[0029] The following are comparative examples of CVI or CVD performed in atmosphere furnaces (tube furnaces or deposition furnaces) based on conventional heating methods: Comparative Example 1 (1) Place the SiC fiber preform in a graphite fixture and then place it in a tube furnace; (2) Seal the tube furnace, evacuate the tube furnace to 10 kPa, start the heating program, and after about 3 hours (the heating rate is about 5 °C / min), the temperature of the tube furnace reaches 1000 °C. During the heating period, the tube furnace is kept at 10 kPa. (3) A mixture of argon, hydrogen and trichloromethylsilane is introduced into a tube furnace to deposit SiC on the fiber surface. The flow rate of the mixed gas is 30 mL / min. (4) After the reaction has been going on for 30 min, turn off the heating program and turn off the mixed gas of hydrogen and trichloromethylsilane. Argon is used as a protective gas with a flow rate of 50 mL / min. (5) Argon gas is continuously introduced into the tube furnace for about 5 hours, cooled to room temperature, and the SiC fiber preform is taken out. (6) The surface microstructure of the SiC fiber in the obtained SiC fiber preform is as follows:Figure 5 As shown, a thin SiC layer can be observed on the fiber surface.

[0030] As can be seen from Comparative Example 1, CVI or CVD deposition of SiC based on the Joule heating principle can greatly improve deposition efficiency, save time and costs, and reduce equipment costs.

Claims

1. An apparatus for preparing fiber-reinforced SiC ceramic matrix composites based on Joule heat chemical vapor infiltration, characterized in that: it comprises a flowing protective gas introduction device (8), a tail gas treatment device (9), a graphite clamp (1), a fiber preform (2), a chloromethylsilane container (3), a reactor, a gas pipe (6) and a valve (7); the reactor is provided with the graphite clamp (1) and the fiber preform (2), the graphite clamp (1) clamps the fiber preform (2), the reactor is connected with a plurality of gas pipes (6), each gas pipe (6) is provided with a corresponding valve (7), and the chloromethylsilane container (3), the flowing protective gas introduction device (8) and the tail gas treatment device (9) are respectively communicated with the reactor through the gas pipe (6).

2. The apparatus for preparing fiber-reinforced SiC ceramic matrix composites based on Joule heat chemical vapor infiltration according to claim 1, characterized in that: the reactor is mainly composed of a quartz tube (4) and metal flanges (5) at both ends of the quartz tube (4) for sealing the quartz tube (4); the graphite clamp (1) has a two-layer structure, and a plurality of holes are distributed on the surfaces of the two layers; the fiber preform (2) contains a plurality of fibers (13) connected with electrodes (11) as heat sources.

3. The apparatus for preparing fiber-reinforced SiC ceramic matrix composites based on Joule heat chemical vapor infiltration according to claim 1, characterized in that: a heating jacket (10) is further arranged on the periphery of the chloromethylsilane container (3), the chloromethylsilane container (3) is internally provided with chloromethylsilane and externally connected with a gas inlet pipe, and a gas inlet valve is correspondingly arranged on the gas inlet pipe.

4. The apparatus for preparing fiber-reinforced SiC ceramic matrix composites based on Joule heat chemical vapor infiltration according to claim 1 or 2, characterized in that: it further comprises a power supply (12), electrodes (11) and wires (14), the power supply (12) is connected to the outside of the reactor through the wires (14), a plurality of fibers (13) are respectively led out from the two ends of the fiber preform (2), one electrode (11) is correspondingly arranged on each metal flange (5) at both ends of the quartz tube (4) of the reactor, each fiber (13) at each end is connected to the electrode (11) of the corresponding metal flange (5) at the same end, and the electrodes (11) of the metal flanges (5) at both ends of the quartz tube (4) of the reactor are respectively connected to the two ends of the power supply (11) through the wires (14). The preparation method comprises: 1) placing the fiber preform (2) in the graphite clamp (1) and placing the graphite clamp (1) in the reactor; 2) connecting each fiber (13) at each end to the electrode (11) of the corresponding metal flange (5) at the same end, then vacuumizing the inside of the reactor and keeping the inside of the reactor in a continuous vacuum state; 3) turning on the power supply (12) to electrify the fiber preform (2) and make the temperature of the fiber preform (2) rise. ​ 5. A method for producing a fiber-reinforced SiC ceramic matrix composite material by Joule heat chemical vapor infiltration using the apparatus according to any one of claims 1 to 4, characterized by, ​ ​ ​ ​ 4) while the trichloromethylsilane container (3) is being heated, the mixed gas of trichloromethylsilane and carrier gas is made to enter the reactor; the gas produced in the reaction process is made to enter the tail gas treatment device (9); 5) after the reaction is completed, the power supply (12) is turned off, the mixed gas of trichloromethylsilane and hydrogen is stopped, the flowing protective gas is made to enter, and the composite material is taken out under the protective atmosphere after cooling to room temperature.

6. The method according to claim 5, wherein the device is used for the preparation of fiber-reinforced SiC ceramic matrix composites by Joule-heating chemical vapor infiltration, and wherein the device is used in the following way: The step 1) is specifically: The fiber preform (2) is placed in the graphite clamp (1), then the metal flanges (5) on both sides of the quartz tube (4) are opened, and the graphite clamp (1) clamping the fiber preform (2) is placed in the reactor; The fiber preform (2) is one of a one-dimensional fiber bundle of SiC fiber, a two-dimensional fiber woven cloth of SiC fiber, a three-dimensional fiber woven body of SiC fiber, a one-dimensional fiber bundle of C fiber, a two-dimensional fiber woven cloth of C fiber, or a three-dimensional fiber woven body of C fiber.

7. The method according to claim 5, wherein the material preparation method of the device for preparing fiber-reinforced SiC ceramic matrix composite based on Joule heating chemical vapor infiltration is characterized by, The step 2) is specifically: Each of the fibers (13) at each end is connected to the electrode (11) of the metal flange (5) at the corresponding end, the metal flanges (5) on both sides of the quartz tube (4) are closed, and the inside of the reactor is vacuumed by a vacuum pump to make the air pressure lower than 15 KPa, and the inside of the reactor is kept in a vacuum state.

8. The material preparation method of the apparatus for preparing fiber-reinforced SiC ceramic matrix composites based on Joule thermochemical vapor infiltration according to claim 5, characterized in that, The step 3) is specifically: The power supply (12) is turned on, and each of the fibers (13) at each end is sequentially electrified by the power supply (12), so that the fiber preform (2) is electrified, and the multiple fiber heat sources in the fiber preform (2) generate heat when electrified, so that the temperature of the fiber preform (2) rises.

9. The method according to claim 5, wherein the device is made of materials selected from the group consisting of stainless steel, carbon steel, and aluminum. The step 4) is specifically: The gas inlet valve outside the trichloromethylsilane container (3) is opened, hydrogen is used as the carrier gas, and the hydrogen is bubbled into the trichloromethylsilane container (3) through the gas inlet pipe by the bubbling method, the heating jacket (10) is started, the trichloromethylsilane container is heated, then the valve (7) of the communication gas pipe (6) between the trichloromethylsilane container (3) and the reactor is opened, so that the mixed gas of trichloromethylsilane and hydrogen enters the reactor; at the same time, the valve (7) of the communication gas pipe (6) between the tail gas treatment device (9) and the reactor is opened, the HCl gas produced in the reaction process is made to enter the tail gas treatment device (9) containing a 5-20wt% NaOH solution, the reaction time is 1-3h, and the reaction temperature is 900-1200℃.

10. A method of producing a fiber-reinforced SiC ceramic matrix composite material based on a device for producing a fiber-reinforced SiC ceramic matrix composite material by Joule heat chemical vapor infiltration according to claim 5, characterized in that, The step 5) is specifically: After the reaction time is completed, the power supply (12) is turned off, the valve (7) of the communication gas pipe (6) between the trichloromethylsilane container (3) and the reactor is closed, the mixed gas of trichloromethylsilane and hydrogen is stopped, the valve (9) of the communication gas pipe (6) between the flowing protective gas inlet device (8) and the reactor is opened, the flowing protective gas is made to enter, the composite material is taken out under the protective gas atmosphere after cooling to room temperature, the metal flanges (5) on both sides of the quartz tube (4) are opened, and the composite material is taken out; The protective gas is argon or nitrogen, and the flow rate is 30-250mL / min.

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