Continuous silicon carbide fiber titanium carbide silicon interface deposition apparatus and method

Abstract

The continuous silicon carbide fiber titanium silicide interface deposition equipment and method of the present application belong to the interface deposition device field, which comprises a closed wire discharge area, a conveying assembly is arranged in the closed wire discharge area, the conveying assembly is used for stress release and continuous conveying of the silicon carbide fiber; a first heat treatment area, a first chemical vapor deposition area, a second chemical vapor deposition area, a second heat treatment area and a closed wire collecting area, a recovery assembly is arranged in the closed wire collecting area, the recovery assembly can release stress and continuously recover the silicon carbide fiber after heat treatment of the second heat treatment area, the situation that the continuous silicon carbide fiber deposition needs to be bent for multiple times is avoided, and the deposition efficiency is improved.

Description

Technical Field

[0001] This invention belongs to the technical field of interface deposition apparatus, and particularly relates to a continuous silicon carbide fiber titanium carbide silicon interface deposition apparatus and method. Background Technology

[0002] Ceramic matrix composites (CMCs), with their ultra-high temperature resistance (up to 1200℃), are currently being used as alternatives to high-temperature alloys in applications such as high-temperature components for aero-engines and cladding tubes for nuclear reactors, requiring extreme temperature resistance and radiation protection. CMCs consist of ceramic fibers, interfaces, and a matrix. Directly introducing ceramic fibers into a ceramic matrix typically results in brittle composites because the strong chemical bonds or frictional resistance between the fibers and the matrix allow matrix cracks to penetrate directly into the fibers. Interface control between the fibers and the matrix plays a crucial role in improving the toughness and damage tolerance of CMCs. Adjustable mechanical and thermal expansion properties, crack deflection, and controlled sliding stress are all important. The choice of interface can enhance the material's high-temperature resistance and radiation resistance. Furthermore, during the densification of CMCs at high temperatures, the matrix precursor may chemically erode the silicon carbide fibers; the interface acts as a barrier to prevent chemical erosion and fiber degradation by blocking the reaction and diffusion of the ceramic fibers.

[0003] The existing process involves depositing BN and its combination coatings on the surface of continuous silicon carbide fibers. These coatings, such as BN / SiC, BN / Si3N4, BN / SiC / C, and BN / Si3N4 / C, have weak oxidation resistance and neutron radiation resistance. Furthermore, the continuous silicon carbide interface coating deposition equipment is complex and difficult to control the continuous deposition of multi-cavity SiC fibers, which makes it difficult to meet the process requirements.

[0004] Existing equipment requires multiple bending operations for continuous silicon carbide fiber deposition, which can easily cause breakage and fiber damage, especially for high-modulus fibers.

[0005] In summary, the existing equipment has low process efficiency for deposition. Summary of the Invention

[0006] The continuous silicon carbide fiber-titanium carbide-silicon carbide interface deposition apparatus provided by this invention solves the technical problem of low interface deposition efficiency in existing devices. The technical solution of this invention has many beneficial effects, as described below:

[0007] A continuous silicon carbide fiber titanium carbide silicon interface deposition equipment includes a closed fiber feeding area with a conveying component inside, the conveying component being used for stress relief and continuous conveying of silicon carbide fibers.

[0008] The first heat treatment zone is provided with a first heating component and is connected to a first argon gas tank. The first heating component can heat the temperature in the heat treatment zone. After argon gas is introduced, the sizing agent on the surface of the silicon carbide fiber conveyed by the conveying component can be removed through the first heating component.

[0009] The first chemical vapor deposition zone is provided with a second heating component and is connected to a first gas supply component. The first gas supply component is capable of supplying a first mixed gas, which is a mixture of argon, titanium tetrachloride and hydrogen, or a mixture of argon, trichloromethylsilane and hydrogen. Under the heating action of the second heating component, a silicon carbide transition layer can be deposited on the surface of the silicon carbide fiber after the sizing agent has been removed.

[0010] The second chemical vapor deposition zone is provided with a third heating component and is connected to a second gas supply component. The second gas supply component can supply a second mixed gas, which is a mixture of argon, titanium tetrachloride and hydrogen. Under the heating action of the third heating component, a titanium carbide-silicon interface can be deposited on the surface of the silicon carbide fiber after the silicon carbide transition layer is deposited.

[0011] The second heat treatment zone is equipped with a fourth heating component and is connected to a second argon gas tank. After argon gas is introduced and heated by the fourth heating component, the silicon carbide fiber after the titanium carbide silicon interface is deposited can be heat treated.

[0012] The sealed take-up area is equipped with a recycling component, which can release stress and continuously recycle the silicon carbide fibers after heat treatment in the second heat treatment zone.

[0013] Compared with the prior art, the technical solution provided by the present invention has the following beneficial effects:

[0014] The vertical interface deposition process enables the uniform unfolding of continuous silicon carbide fiber bundles, which continuously pass through the multi-cavity chemical vapor deposition zone and heat treatment zone, completing the fiber feeding and winding within one cycle. This effectively reduces the damage caused by repeated bending of silicon carbide fibers, thereby improving the deposition efficiency. Attached Figure Description

[0015] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0016] Figure 1 This is a schematic diagram illustrating the processing of the device of the present invention;

[0017] Figure 2 A schematic diagram of a closed yarn feeding area and a closed yarn taking area;

[0018] Figure 3 A schematic diagram of the first heat treatment zone and the first chemical vapor deposition zone;

[0019] Figure 4 This is a schematic diagram of the second chemical vapor deposition zone and the second heat treatment zone, wherein...

[0020] 1. Sealed yarn feeding area; 2. First heat treatment area; 3. First chemical vapor deposition area; 4. First argon gas isolation area; 5. Second chemical vapor deposition area; 6. Second argon gas isolation area; 7. Second heat treatment area; 8. Sealed yarn taking area; 9. Third argon gas isolation area; 91. Liquid nitrogen cooling trap; 92. Adsorption molecular sieve; 93. Vacuum pump; 94. Spray tower; 101. First argon gas tank; 102. Second argon gas tank; 103. Third argon gas tank; 104. Fourth argon gas tank; 11. Yarn feeding bobbin; 12. First large yarn guide roller; 13. First small yarn guide roller; 14. First... 21. Pressing roller; 22. First graphite heating element; 23. First thermocouple; 24. First air inlet pipe; 31. Second graphite heating element; 32. Second thermocouple; 33. Second air inlet pipe; 34. Second air outlet pipe; 51. Third graphite heating element; 52. Third thermocouple; 53. Third air inlet pipe; 54. Third air outlet pipe; 71. Fourth graphite heating element; 72. Fourth thermocouple; 73. Fourth air inlet pipe; 74. Fourth air outlet pipe; 81. Take-up bobbin; 82. Second large yarn guide roller; 83. Second small yarn guide roller; 84. Second pressing roller. Detailed Implementation

[0021] The following specific examples illustrate the implementation of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention. It should be noted that, in the absence of conflict, the following embodiments and features in the embodiments can be combined with each other. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0022] It should be noted that various aspects of embodiments within the scope of the appended claims are described below. It will be apparent that the aspects described herein can be embodied in a wide variety of forms, and any particular structure and / or function described herein is merely illustrative. Based on this invention, those skilled in the art will understand that one aspect described herein can be implemented independently of any other aspect, and two or more of these aspects can be combined in various ways. For example, any number of aspects set forth herein can be used to implement the device and / or practice the method. Additionally, this device and / or method can be implemented using structures and / or functionalities other than one or more of the aspects set forth herein.

[0023] It should also be noted that the illustrations provided in the following embodiments are only schematic representations of the basic concept of the present invention. The drawings only show the components related to the present invention and are not drawn according to the actual number, shape and size of the components in the actual implementation. In the actual implementation, the form, quantity and proportion of each component can be arbitrarily changed, and the layout of the components may also be more complex.

[0024] Furthermore, specific details are provided in the following description to facilitate a thorough understanding of the examples. However, those skilled in the art will understand that aspects can be practiced without these specific details. To enable those skilled in the art to better understand the invention, the invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. The terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, features defined as "first" and "second" may explicitly or implicitly include one or more of that feature. In the description of the invention, unless otherwise stated, "a plurality of" means two or more.

[0025] like Figures 1 to 4 The continuous silicon carbide fiber-titanium carbide-silicon interface deposition equipment shown includes a sizing agent formed on the surface of the silicon carbide fiber during the initial preparation process. The titanium carbide-silicon has the chemical formula Ti3SiC2 and comprises...

[0026] The sealed fiber feeding area 1 is equipped with a conveying assembly, which is used for stress relief and continuous conveying of silicon carbide fibers.

[0027] The first heat treatment zone 2 is provided with a first heating component and is connected to a first argon gas tank 101. The first heating component can heat the temperature in the heat treatment zone. After argon gas is introduced, the sizing agent on the surface of the silicon carbide fiber conveyed by the conveying component can be removed through the first heating component.

[0028] A first chemical vapor deposition zone 3 is provided within which a second heating component is connected to a first gas delivery component. The first gas delivery component delivers a first mixed gas, which is either a mixture of argon, titanium tetrachloride, and hydrogen, or a mixture of argon, trichloromethylsilane, and hydrogen. Heated by the second heating component, a silicon carbide transition layer is deposited on the surface of the silicon carbide fiber after the sizing agent has been removed. The first mixed gas is prepared, for example, by using a mixing tank connected to a hydrogen tank, a trichloromethylsilane tank, and an argon tank. An additional valve is provided between the hydrogen tank and the trichloromethylsilane tank to control the flow rate or molar ratio of the first mixed gas.

[0029] The second chemical vapor deposition zone 5 is equipped with a third heating component and is connected to a second gas supply component. The second gas supply component can supply a second mixed gas, which is a mixture of argon, titanium tetrachloride and hydrogen. Under the heating action of the third heating component, a titanium carbide-silicon interface can be deposited on the surface of the silicon carbide fiber after the silicon carbide transition layer is deposited. The second mixed gas can be prepared, for example, by using a gas mixing tank connected to a hydrogen tank, a titanium tetrachloride tank and an argon tank. The principle is the same as that of the preparation of the first gas supply component.

[0030] The second heat treatment zone 7 is equipped with a fourth heating component and is connected to a second argon gas tank 102. After argon gas is introduced and heated by the fourth heating component, the silicon carbide fiber after the titanium carbide silicon interface is deposited can be heat treated.

[0031] The sealed take-up zone 8 is equipped with a recycling component, which can release stress and continuously recycle the silicon carbide fibers after heat treatment in the second heat treatment zone 7.

[0032] Preferably, each of the above-mentioned zones has a wire hole at the corresponding position to facilitate the feeding of silicon carbide fibers and prevent deviation during the feeding process. The continuous silicon carbide fibers move from the bottom sealed feeding zone 1 to the top sealed receiving zone 8. The gases in each deposition and heat treatment zone enter the working area from the top and flow out of the working area from the bottom, thereby achieving good temperature uniformity and deposition uniformity.

[0033] Furthermore, the various zones of the aforementioned device can be applied to existing chemical furnaces to form an integrated unit, which can improve deposition efficiency.

[0034] In one embodiment, a first argon gas isolation zone 4 is provided between the first chemical vapor deposition zone 3 and the second chemical vapor deposition zone 5, and a second argon gas isolation zone 6 is provided between the second chemical vapor deposition zone 5 and the second heat treatment zone 7.

[0035] The first argon isolation zone 4 is connected to the third argon tank 103. Argon gas in the third argon tank 103 is input into the first argon isolation zone 4, so that the pressure in the first argon isolation zone 4 is higher than the pressure in the first chemical vapor deposition zone 3 and the second chemical vapor deposition zone 5, for example, 100-200 Pa higher, to ensure that the first mixed gas does not flow out.

[0036] The second argon isolation zone 6 is connected to the fourth argon tank 104. Argon gas in the fourth argon tank 104 is input into the second argon isolation zone 6, so that the pressure in the second argon isolation zone 6 is higher than the pressure in the second chemical vapor deposition zone 5 and the second heat treatment zone 7, for example, 100-200 Pa higher, to ensure that the second mixed gas does not flow out.

[0037] Furthermore, a third argon gas isolation zone 9 is provided between the second heat treatment zone 7 and the sealed winding zone 8. The third argon gas isolation zone 9 is also equipped with an argon gas tank and an inlet pipe and an outlet pipe to control the pressure in the third argon gas isolation zone 9.

[0038] In one embodiment, considering environmental protection, an exhaust gas treatment component is also included. This component comprises a liquid nitrogen cooling trap 91, an adsorption molecular sieve 92, a vacuum pump 93, and a spray tower 94.

[0039] The exhaust gases from the first argon isolation zone 4, the second argon isolation zone 6, the first heat treatment zone 2, the second heat treatment zone 7, the first chemical vapor deposition zone 3, and the second chemical vapor deposition zone 5 are all transported through pipelines to the liquid nitrogen cooling trap 91 for partial condensation. The remaining exhaust gases that are not condensed are transported to the adsorption molecular sieve 92 for secondary filtration, and then, after passing through the vacuum pump 93, the remaining exhaust gases are transported to the spray tower 94 for spraying before being directly discharged, without causing pollution to the environment or atmosphere.

[0040] In one embodiment, the sealed fiber feeding zone 1 is located below the sealed fiber receiving zone 8. The silicon carbide fibers conveyed in the sealed fiber feeding zone 1 pass through the first heat treatment zone 2, the first chemical vapor deposition zone 3, the first argon gas isolation zone 4, the second chemical vapor deposition zone 5, the second argon gas isolation zone 6, and the second heat treatment zone 7 in sequence before being recovered by the recovery component. The deposition is carried out in a vertical manner, which utilizes the physical properties of the gas to improve the deposition efficiency and the efficiency of exhaust gas discharge.

[0041] In one embodiment, the conveying assembly includes a feeding spool 11, a first large guide roller 12, a first small guide roller 13, and a first pressure roller 14; the recovery assembly includes a take-up spool 81, a second large guide roller 82, a second small guide roller 83, and a second pressure roller 84. Preferably, the feeding spool 11 and the take-up spool 81 simultaneously feed and take up multiple carbon fibers.

[0042] The yarn feeding spool 11 is installed on the output end of the first motor and is wound with silicon carbide fibers. The silicon carbide fibers are released under the rotation of the first large yarn guide roller 12, and after being oriented by the first small yarn guide roller 13, they are conveyed to a pair of first yarn pressing rollers 14 for widening to a preset width (controlled between 10-40μm). After widening, they are conveyed to the first heat treatment zone 2 for heat treatment.

[0043] After being treated in the second heat treatment zone 7, the silicon carbide fibers are widened to a preset width by a pair of second pressing rollers 84 and oriented by the second small guide rollers 83. They are then conveyed to the second large guide rollers 82 for stress release and are taken back by the take-up drum 81, which is installed on the output end of the second motor.

[0044] Furthermore, it also includes a controller, and the first heating assembly includes a first graphite heating element 21, a first thermocouple 22, a first air inlet pipe 23, and a first air outlet pipe 24, wherein,

[0045] The first graphite heating element 21 is electrically connected to a DC power supply, which can heat the first heat treatment zone 2 to 1400°C. The DC power supply and the first thermocouple 22 are both electrically connected to the controller.

[0046] The first thermocouple 22 is installed by a support frame and is 10±2mm away from the silicon carbide fiber. It can collect the temperature of the silicon carbide fiber and feed it back to the controller, so that the controller can control the heat generation of the first graphite heating element 21.

[0047] Argon gas in the first argon tank 101 can enter the first heat treatment zone 2 through the first inlet pipe 23 and be discharged through the first outlet pipe 24.

[0048] Furthermore, the second heating assembly includes a second graphite heating element 31, a second thermocouple 32, a second air inlet pipe 33, and a second air outlet pipe 34, wherein,

[0049] The second graphite heating element 31 is connected to a DC power supply, which can heat the first chemical vapor deposition region 3 to 1400°C. The DC power supply and the second thermocouple 32 are both electrically connected to the controller.

[0050] The second thermocouple 32 is installed via a support frame and is 10±2mm away from the silicon carbide fiber. It can collect the temperature of the silicon carbide fiber and feed it back to the controller, so that the controller can control the heat generation of the second graphite heating element 31.

[0051] The first mixed gas can enter the first chemical vapor deposition zone 3 through the second inlet pipe 33 and be discharged through the second outlet pipe 34;

[0052] The third heating assembly includes a third graphite heating element 51, a third thermocouple 52, a third air inlet pipe 53, and a third air outlet pipe 54, wherein...

[0053] The third graphite heating element 51 is connected to a DC power supply, which can heat the second chemical vapor deposition region 5 to 1400°C. The DC power supply and the third thermocouple 52 are both electrically connected to the controller.

[0054] The third thermocouple 52 is installed via a support frame and is 10±2mm away from the silicon carbide fiber. It can collect the temperature of the silicon carbide fiber and feed it back to the controller, so that the controller can control the heat generation of the third graphite heating element 51.

[0055] The second mixed gas can enter the second chemical vapor deposition zone 5 through the third inlet pipe 53 and be discharged through the third outlet pipe 54.

[0056] Furthermore, the fourth heating assembly includes a fourth graphite heating element 71, a fourth thermocouple 72, a fourth air inlet pipe 73, and a fourth air outlet pipe 74, wherein,

[0057] The fourth graphite heating element 71 is connected to a DC power supply, which can heat the second heat treatment zone 7 to 1600℃. The DC power supply and the fourth thermocouple 72 are both electrically connected to the controller.

[0058] The fourth thermocouple 72 is installed via a support frame and is 10±2mm away from the silicon carbide fiber. It can collect the temperature of the silicon carbide fiber and feed it back to the controller, so that the controller can control the heat generation of the fourth graphite heating element 71.

[0059] Argon gas in the second argon tank 102 can enter the second heat treatment zone 7 through the fourth inlet pipe 73 and be discharged through the fourth outlet pipe 74. Preferably, the first pressing roller 14 and the second pressing roller 84 are perpendicular to each other, which effectively avoids tensile damage to the continuous silicon carbide fibers.

[0060] Preferably, the aforementioned multiple graphite heating elements are arranged in a barrel-like structure.

[0061] Secondly, a continuous silicon carbide fiber-titanium carbide-silicon interface deposition method is provided, using some or all of the above-described continuous silicon carbide fiber-titanium carbide-silicon interface deposition equipment, the method comprising:

[0062] Step 1: Use vacuum pump 93 to evacuate the sealed wire feeding area 1, the first heat treatment area 2, the first chemical vapor deposition area 3, the first argon isolation area 4, the second chemical vapor deposition area 5, the second argon isolation area 6, the second heat treatment area 7 and the sealed wire taking area 8. The pressure is below 50 Pa, and the pressure is maintained for 1 hour with a pressure rise rate ≤ 100 Pa / h.

[0063] Step 2: After vacuum pressure holding, argon gas is introduced into the sealed wire feeding area 1, the first heat treatment area 2, the first chemical vapor deposition area 3, the first argon gas isolation area 4, the second chemical vapor deposition area 5, the second argon gas isolation area 6, the second heat treatment area 7 and the sealed wire taking area 8 respectively, and the pressure is controlled at 200-1000 Pa.

[0064] In the first heat treatment zone 2, the first chemical vapor deposition zone 3, the second chemical vapor deposition zone 5, and the second heat treatment zone 7, direct current is applied to the graphite heating elements to begin heating.

[0065] The temperature in the first heat treatment zone 2 is controlled at 600-800℃;

[0066] The temperature in the first chemical vapor deposition zone 3 is controlled at 1050–1150℃;

[0067] The temperature in the second chemical vapor deposition zone 5 is controlled at 1050–1200℃;

[0068] The temperature of the second heat treatment zone 7 is controlled at 1200-1600℃;

[0069] Step 3: A first mixed gas is introduced into the first chemical vapor deposition zone 3, wherein the hydrogen flow rate ranges from 4 to 40 L / min. -1 Argon flow rate is 1–10 L / min -1 And the deposition pressure is controlled at 300–2000 Pa;

[0070] The second chemical vapor deposition zone 5 is introduced with a second mixed gas, wherein the hydrogen flow rate is 4–25 L / min. -1 Argon flow rate is 5–50 L / min -1 During the deposition process, the molar ratio of hydrogen to titanium tetrachloride is controlled at 5–20, and the deposition pressure is controlled at 300–2000 Pa.

[0071] Argon gas is continuously supplied to the first argon isolation zone 4 and the second argon isolation zone 6, so that the pressure in the first argon isolation zone 4 is 50-100 Pa higher than the pressure in the first chemical vapor deposition zone 3; and the pressure in the second argon isolation zone 6 is 50-100 Pa higher than the pressure in the second chemical vapor deposition zone 5.

[0072] Step 3: The feeding drum 11 on the first motor and the taking drum 81 on the second motor start synchronously to ensure the feeding speed of the silicon carbide fiber and to ensure that the silicon carbide fiber has tension in the vertical direction and does not bend. The feeding speed of the silicon carbide fiber is 1 to 3 m / min, and the taking speed of the taking drum 81 is 1% to 10% faster than the feeding speed of the feeding drum 11.

[0073] The core of the above process is as follows: First, continuous silicon carbide fibers are heated to the deposition temperature (800-1000℃) in an inert atmosphere to remove the sizing agent. Second, the continuous silicon carbide fibers enter two independent deposition zones. In the first deposition zone, a first mixed gas is introduced, in which trichloromethylsilane serves as both the silicon and carbon source, and hydrogen and argon serve as dilution gases. Trichloromethylsilane is introduced into the first chemical vapor deposition zone 3, and after a certain time, the SiC transition interface layer prepared has a thickness of 100-800 nm. Finally, a second mixed gas is introduced into the second chemical vapor deposition zone 5. The second mixed gas is a reaction mixture of titanium tetrachloride (TiCl4), hydrogen, and argon, in which titanium tetrachloride serves as the titanium source, and hydrogen and argon serve as dilution gases. Titanium tetrachloride is transported into the second chemical vapor deposition zone 5, and after deposition on the surface of the transition silicon carbide interface layer, the final titanium carbide silicon interface layer prepared has a thickness of 150-1000 nm.

[0074] The deposition reaction is reactive chemical vapor deposition:

[0075] 2SiC(s)+3TiCl4(g)+5H2(g)→Ti3SiC2(s)+SiCl2(g)+10HCl(g)

[0076] This method effectively deposits a titanium-silicon carbide interface layer of a specific thickness on the surface of continuous silicon carbide fibers and preforms through in-situ deposition. The low deposition temperature effectively reduces damage to the silicon carbide fibers caused by prolonged deposition, significantly improving the high-temperature resistance and radiation resistance of the interface layer. The deposited continuous silicon carbide fibers can be used for prepreg preparation, meeting the requirements of prepreg-melt infiltration processes for preparing ceramic matrix composites. Furthermore, this in-situ deposition method can also accommodate interface deposition of preforms with different structures and sizes, allowing for efficient integration of interface deposition with subsequent densification processes (such as melt infiltration and resin impregnation pyrolysis). This enhances the temperature resistance and radiation resistance of ceramic matrix composites prepared using this interface layer densification. Additionally, the process allows for control of parameters in various regions. The thickness of the interface layer, for example,

[0077] 1) Vacuuming of each zone: Pressure below 50 Pa, pressure held for 1 hour, and pressure rise rate ≤ 100 Pa / h. Argon gas is then introduced into each zone, with pressure controlled at 200-500 Pa. The temperature of the first heat treatment zone 2 is controlled at 700-750℃, the temperature of the first chemical vapor deposition zone 3 is controlled at 1070-1100℃, the temperature of the second chemical vapor deposition zone 5 is controlled at 1080-1120℃, and the temperature of the second heat treatment zone 7 is controlled at 1400-1450℃. The first chemical vapor deposition zone 3 is introduced with a first mixed gas (hydrogen flow rate range of 8-12 L·min). -1 Argon flow rate is 2–6 L / min -1The deposition pressure is controlled at 800–1200 Pa, and a second mixed gas (hydrogen flow rate of 5–8 L / min) is introduced into the second chemical vapor deposition zone 5. -1 Argon flow rate is 2–6 L / min -1 During the deposition process, the molar ratio of hydrogen to titanium tetrachloride is 5-8, and the deposition pressure is controlled at 800-1200 Pa. Argon gas is continuously introduced into the first argon isolation zone 4 and the second argon isolation zone 6, so that the pressure of the first argon isolation zone 4 is 50-100 Pa higher than the pressure of the first chemical vapor deposition zone 3, and the pressure of the second argon isolation zone 6 is 50-100 Pa higher than the pressure of the second chemical vapor deposition zone 5. The thickness of the silicon carbide fiber bundle after expansion is 15-20 μm, the fiber feeding speed is 2±0.2 m / min, the fiber take-up speed is 2%-3% faster than the fiber release speed, and the thickness of the titanium carbide silicon interface obtained on the surface of the continuous silicon carbide fiber is 300-400 nm.

[0078] 2) Vacuuming of each zone: Pressure is reduced to below 50 Pa, maintained for 1 hour, and pressure rise rate ≤ 100 Pa / h. Argon gas is then introduced into each zone, with pressure controlled at 200-500 Pa. The temperature of the first heat treatment zone 2 is controlled at 700-750℃, the first chemical vapor deposition zone 3 at 1070-1100℃, the second chemical vapor deposition zone 5 at 1080-1120℃, and the second heat treatment zone 7 at 1400-1450℃. A first mixed gas (hydrogen flow rate range of 24-28 L / min) is introduced into the first chemical vapor deposition zone 3. -1 Argon flow rate is 6-7 L / min -1 The deposition pressure is controlled at 800–1200 Pa, and a second mixed gas (hydrogen flow rate of 12–16 L / min) is introduced into the second chemical vapor deposition zone 5. -1 Argon flow rate is 15–20 L / min -1 During the deposition process, the molar ratio of hydrogen to titanium tetrachloride is 7–10, and the deposition pressure is controlled at 800–1200 Pa. Argon gas is continuously introduced into the first argon isolation zone 4 and the second argon isolation zone 6, so that the pressure of the first argon isolation zone 4 is 50–00 Pa higher than the pressure of the first chemical vapor deposition zone 3, and the pressure of the second argon isolation zone 6 is 50–100 Pa higher than the pressure of the second chemical vapor deposition zone 5. The thickness of the broadened silicon carbide fiber bundle is 15–20 μm, the fiber feeding speed is 2 ± 0.2 m / min, and the take-up speed is 2%–3% faster than the release speed. Finally, the thickness of the titanium carbide-silicon interface obtained on the surface of the continuous silicon carbide fiber is 400–500 nm.

[0079] This article uses specific examples to illustrate the principles and implementation methods of the present invention. The descriptions of the above embodiments are only for the purpose of helping to understand the core ideas of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made to the invention without departing from the principles of the invention, and these improvements and modifications also fall within the protection scope of the invention claims.

Claims

1. A continuous silicon carbide fiber titanium carbide silicon interface deposition apparatus, characterized in that, include, A closed yarn feeding area is provided with a conveying assembly, which is used for stress relief and continuous conveying of silicon carbide fibers. The conveying assembly includes a yarn feeding cylinder, a first large yarn guide roller, a first small yarn guide roller, and a first yarn pressing roller. The first heat treatment zone is provided with a first heating component and is connected to a first argon gas tank. The first heating component can heat the temperature in the heat treatment zone. After argon gas is introduced, the sizing agent on the surface of the silicon carbide fiber conveyed by the conveying component can be removed through the first heating component. The first chemical vapor deposition zone is provided with a second heating component and is connected to a first gas supply component. The first gas supply component is capable of supplying a first mixed gas, which is a mixture of argon, trichloromethylsilane and hydrogen. Under the heating action of the second heating component, a silicon carbide transition layer can be deposited on the surface of the silicon carbide fiber after the sizing agent has been removed. The second chemical vapor deposition zone is provided with a third heating component and is connected to a second gas supply component. The second gas supply component can supply a second mixed gas, which is a mixture of argon, titanium tetrachloride and hydrogen. Under the heating action of the third heating component, a titanium carbide-silicon interface can be deposited on the surface of the silicon carbide fiber after the silicon carbide transition layer is deposited. The second heat treatment zone is equipped with a fourth heating component and is connected to a second argon gas tank. After argon gas is introduced and heated by the fourth heating component, the silicon carbide fiber after the titanium carbide silicon interface is deposited can be heat treated. The sealed take-up area is equipped with a recycling component, which can release stress and continuously recycle the silicon carbide fibers after heat treatment in the second heat treatment zone. The closed fiber feeding area is located below the closed fiber receiving area. The silicon carbide fibers conveyed in the closed fiber feeding area pass through the first heat treatment area, the first chemical vapor deposition area, the first argon isolation area, the second chemical vapor deposition area, the second argon isolation area, and the second heat treatment area in sequence before being recovered by the recovery component. The recycling assembly includes a take-up bobbin, a second large yarn guide roller, a second small yarn guide roller, and a second yarn pressing roller.

2. The continuous silicon carbide fiber titanium carbide silicon interface deposition equipment according to claim 1, characterized in that, A first argon gas isolation zone is provided between the first chemical vapor deposition zone and the second chemical vapor deposition zone, and a second argon gas isolation zone is provided between the second chemical vapor deposition zone and the second heat treatment zone. The first argon gas isolation zone is connected to a third argon gas tank. Argon gas from the third argon gas tank is input into the first argon gas isolation zone, so that the pressure in the first argon gas isolation zone is higher than the pressure in the first chemical vapor deposition zone and the second chemical vapor deposition zone. The second argon gas isolation zone is connected to a fourth argon gas tank. Argon gas from the fourth argon gas tank is input into the second argon gas isolation zone, making the pressure in the second argon gas isolation zone higher than the pressure in the second chemical vapor deposition zone and the second heat treatment zone.

3. The continuous silicon carbide fiber titanium carbide silicon interface deposition equipment according to claim 2, characterized in that, It also includes an exhaust gas treatment component, which comprises a liquid nitrogen cooling trap, an adsorption molecular sieve, a vacuum pump, and a spray tower, wherein... The tail gas in the first argon gas isolation zone, the second argon gas isolation zone, the first heat treatment zone, the second heat treatment zone, the first chemical vapor deposition zone, and the second chemical vapor deposition zone is transported to the liquid nitrogen cooling trap for partial condensation. The tail gas that is not condensed is transported to the adsorption molecular sieve for secondary filtration, and after passing through the vacuum pump, the remaining tail gas is transported to the spray tower for spraying and then directly discharged.

4. The continuous silicon carbide fiber titanium carbide silicon interface deposition equipment according to claim 2, characterized in that, The yarn feeding spool is installed on the output end of the first motor and is wound with silicon carbide fibers. The silicon carbide fibers are released under the rotation of the first large yarn guide roller, and after being oriented by the first small yarn guide roller, they are conveyed to a pair of first yarn pressing rollers for widening to a preset width. After widening, they are conveyed to the first heat treatment zone for heat treatment. After being treated in the second heat treatment zone, the silicon carbide fibers are widened to a preset width by a pair of second pressing rollers and oriented by the second small guide rollers. They are then conveyed to the second large guide roller for stress release and are recovered by the take-up drum, which is installed on the output end of the second motor.

5. The continuous silicon carbide fiber titanium carbide silicon interface deposition equipment according to claim 4, characterized in that, It also includes a controller, and the first heating assembly includes a first graphite heating element, a first thermocouple, a first air inlet pipe, and a first air outlet pipe, wherein, The first graphite heating element is electrically connected to a DC power supply, which can heat the first heat treatment zone to 1400°C. The DC power supply and the first thermocouple are both electrically connected to the controller. The first thermocouple is installed by a support frame and is 10±2mm away from the silicon carbide fiber. It can collect the temperature of the silicon carbide fiber and feed it back to the controller, so that the controller can control the heat generation of the first graphite heating element. Argon gas in the first argon tank can enter the first heat treatment zone through the first inlet pipe and be discharged through the first outlet pipe.

6. The continuous silicon carbide fiber titanium carbide silicon interface deposition equipment according to claim 5, characterized in that, The second heating assembly includes a second graphite heating element, a second thermocouple, a second air inlet pipe, and a second air outlet pipe, wherein, The second graphite heating element is connected to a DC power supply, which can heat the first chemical vapor deposition region to 1400°C. The DC power supply and the second thermocouple are both electrically connected to the controller. The second thermocouple is installed via a support frame and is 10±2mm away from the silicon carbide fiber. It can collect the temperature of the silicon carbide fiber and feed it back to the controller, so that the controller can control the heat generation of the second graphite heating element. The first mixed gas can enter the first chemical vapor deposition zone through the second inlet pipe and be discharged through the second outlet pipe; The third heating assembly includes a third graphite heating element, a third thermocouple, a third air inlet pipe, and a third air outlet pipe, wherein... The third graphite heating element is connected to a DC power supply, which can heat the second chemical vapor deposition region to 1400°C. The DC power supply and the third thermocouple are both electrically connected to the controller. The third thermocouple is installed via a support frame and is 10±2mm away from the silicon carbide fiber. It can collect the temperature of the silicon carbide fiber and feed it back to the controller, so that the controller can control the heat generation of the third graphite heating element. The second mixed gas can enter the second chemical vapor deposition zone through the third inlet pipe and be discharged through the third outlet pipe.

7. The continuous silicon carbide fiber titanium carbide silicon interface deposition equipment according to claim 6, characterized in that, The fourth heating assembly includes a fourth graphite heating element, a fourth thermocouple, a fourth air inlet pipe, and a fourth air outlet pipe, wherein... The fourth graphite heating element is connected to a DC power supply, which can heat the second heat treatment zone to 1600°C. The DC power supply and the fourth thermocouple are both electrically connected to the controller. The fourth thermocouple is installed via a support frame and is 10±2mm away from the silicon carbide fiber. It can collect the temperature of the silicon carbide fiber and feed it back to the controller, so that the controller can control the heat generation of the fourth graphite heating element. Argon gas in the second argon tank can enter the second heat treatment zone through the fourth inlet pipe and be discharged through the fourth outlet pipe.

8. A method for continuous silicon carbide fiber-titanium carbide-silicon carbide interface deposition, characterized in that, The continuous silicon carbide fiber titanium carbide silicon interface deposition apparatus as described in claim 7 is used.

9. The continuous silicon carbide fiber titanium carbide silicon interface deposition method according to claim 8, characterized in that, Its methods include, Step 1: Use a vacuum pump to evacuate the sealed wire feeding area, the first heat treatment area, the first chemical vapor deposition area, the first argon isolation area, the second chemical vapor deposition area, the second argon isolation area, the second heat treatment area, and the sealed wire taking area. The pressure should be below 50 Pa, and the pressure should be maintained for 1 hour with a pressure rise rate ≤ 100 Pa / h. Step 2: After vacuum pressure holding, argon gas is introduced into the sealed wire feeding area, the first heat treatment area, the first chemical vapor deposition area, the first argon gas isolation area, the second chemical vapor deposition area, the second argon gas isolation area, the second heat treatment area and the sealed wire taking area respectively, and the pressure is controlled at 200-1000 Pa. Direct current is applied to the graphite heating elements in the first heat treatment zone, the first chemical vapor deposition zone, the second chemical vapor deposition zone, and the second heat treatment zone to begin heating. The temperature in the first heat treatment zone is controlled at 600–800℃; The temperature in the first chemical vapor deposition zone is controlled at 1050–1150℃; The temperature in the second chemical vapor deposition zone is controlled at 1050–1200℃; The temperature in the second heat treatment zone is controlled at 1200–1600℃; Step 3: A first mixed gas is introduced into the first chemical vapor deposition zone, wherein the hydrogen flow rate ranges from 4 to 40 L / min. -1 Argon flow rate is 1–10 L / min -1 And the deposition pressure is controlled at 300–2000 Pa; A second mixed gas is introduced into the second chemical vapor deposition zone, wherein the hydrogen flow rate is 4–25 L / min. -1 Argon flow rate is 5–50 L / min -1 During the deposition process, the molar ratio of hydrogen to titanium tetrachloride is controlled at 5–20, and the deposition pressure is controlled at 300–2000 Pa. Argon gas is continuously supplied to the first argon gas isolation zone and the second argon gas isolation zone respectively, so that the pressure in the first argon gas isolation zone is 50-100 Pa higher than the pressure in the first chemical vapor deposition zone; the pressure in the second argon gas isolation zone is 50-100 Pa higher than the pressure in the second chemical vapor deposition zone. Step 4: The feeding drum on the first motor and the take-up drum on the second motor start synchronously to ensure the feeding speed of the silicon carbide fiber and to ensure that the silicon carbide fiber has tension in the vertical direction and does not bend. The feeding speed of the silicon carbide fiber is 1-3 m / min, and the take-up speed of the take-up drum is 1%-10% faster than the feeding speed of the feeding drum.

Images