A device for continuous vapor deposition wire feeding

Abstract

A device for continuous vapor deposition wire feeding, wherein an atmosphere inlet and a wire inlet are provided at one end of a quartz tube, and an exhaust gas outlet and a wire outlet are provided at the other end; the middle part of the inner cavity of the quartz tube is a reaction zone, and the reaction zone of the quartz tube is arranged in the heating area of ​​a tubular furnace body; the atmosphere inlet of the quartz tube is connected with the outlet of an atmosphere introduction device through a pipeline, and the exhaust gas outlet of the quartz tube is connected with the inlet of an exhaust gas treatment device through a pipeline; the liquid seal box comprises a front liquid seal box and a rear liquid seal box, the wire inlet of the quartz tube is arranged below the liquid level of the front liquid seal box, and the wire outlet of the quartz tube is arranged below the liquid level of the rear liquid seal box; a guide wheel mechanism controls the fiber to be processed to be introduced from the wire inlet of the quartz tube and led out from the wire outlet; the device has a simple structure, can be continuously produced, and can improve the dielectric properties and mechanical properties of the fiber to be processed, and has good application prospects in the fields of absorbing materials, composite material reinforcement, etc.

Description

Technical Field

[0001] The invention belongs to the field of composite fiber preparation and relates to a device for continuous vapor deposition wire feeding. Background Art

[0002] Chemical vapor deposition (CVD) is a method that uses chemical gases or vapors to react on the surface of a substrate to synthesize coatings or nanomaterials and deposit carbon-based materials. It is most widely used in the semiconductor industry and is also used in the reinforcement of composite fiber materials and the preparation of absorbing fiber materials.

[0003] In New Carbon Materials, 2020, 35(4):428-435, an iron-coated carbon nanotube composite absorber was prepared based on metal organic chemical vapor deposition. The morphology and wave absorption properties of the material can be controlled by changing the deposition temperature. In Advanced Electronic Materials, 2018, 4(5):1700565, carbon nanotubes were grown on the surface of activated carbon hollow porous fibers (ACHFs) by chemical vapor deposition, and a multilayer structure of ACHFs-CNTs-Fe3O4 composite absorber was obtained. It can be seen that chemical vapor deposition is widely used in composite fiber reinforcement. However, the floating catalyst method used in the prior art is too expensive, and since there is no continuous preparation equipment in the prior art, it is difficult to meet the stable atmosphere conditions while wire feeding, and it is even more impossible to prepare composite fibers by continuous CVD. Summary of the invention

[0004] The invention solves the shortcomings of the prior art and provides a device for continuous vapor deposition wire feeding which can produce continuously and improve the dielectric property and mechanical property of the fiber to be processed.

[0005] To achieve the above-mentioned purpose, the present invention first proposes a device for continuous vapor deposition wire feeding, including a quartz tube, a guide wheel mechanism, a liquid seal box, an atmosphere introduction device and an exhaust gas treatment device, wherein one end of the quartz tube is provided with an atmosphere inlet and a wire inlet, and the other end is provided with an exhaust gas outlet and a wire outlet, the middle part of the inner cavity of the quartz tube is a reaction zone, the reaction zone of the quartz tube is arranged in the heating area of ​​the tubular furnace body, the atmosphere inlet of the quartz tube is connected with the outlet of the atmosphere introduction device through a pipeline, the exhaust gas outlet of the quartz tube is connected with the inlet of the exhaust gas treatment device through a pipeline, the liquid seal box includes a front liquid seal box and a rear liquid seal box, the wire inlet of the quartz tube is arranged below the liquid level of the front liquid seal box, and the wire outlet of the quartz tube is arranged below the liquid level of the rear liquid seal box; the guide wheel mechanism introduces the fiber to be treated from the wire inlet of the quartz tube, passes through the reaction zone in the middle of the inner cavity of the quartz tube, and leads it out from the wire outlet.

[0006] Through the above structure, on the one hand, the guide wheel mechanism is used to control the fiber to be processed to be introduced from the wire inlet of the quartz tube, pass through the reaction zone in the middle of the inner cavity of the quartz tube, and be led out from the wire outlet; on the other hand, the atmosphere ratio and atmosphere type in the quartz tube are set by the atmosphere introduction device, the reaction temperature of the reaction zone of the quartz tube is set by the tubular furnace body, and the closed environment required for continuous wire feeding reaction is created by the front liquid sealing box and the rear liquid sealing box. Through the coordinated cooperation of the above structures, the continuous production of carbon nanotube modified fibers with specific morphology is realized, thereby improving the dielectric properties and mechanical properties of the fiber to be processed; so that the device has good application prospects in the fields of absorbing materials, composite material reinforcement, etc.

[0007] In this embodiment, the two ends of the quartz tube are respectively provided with a wire inlet tube and a wire outlet tube arranged perpendicularly to the quartz tube, the wire inlet tube and the wire outlet tube are connected to the inner cavity of the quartz tube, one end of the wire inlet tube and the wire outlet tube are sealed with the quartz tube, and the other end forms the wire inlet and the wire outlet, and the wire inlet tube and the wire outlet at both ends of the quartz tube are respectively arranged below the liquid level in the front liquid seal box and the rear liquid seal box.

[0008] In this embodiment, it also includes a wire unwinding machine and a wire collecting machine, the wire unwinding machine is arranged on the side of the wire inlet of the quartz tube, and the wire collecting machine is arranged on the side of the wire outlet of the quartz tube, the wire unwinding machine includes a wire unwinding wheel driven to rotate by a first driving device, and the wire collecting machine includes a wire collecting wheel driven to rotate by a second driving device, the wire unwinding wheel is wound with fibers to be processed, one end of the fibers to be processed is fixed on the wire unwinding wheel, and the other end passes through the wire inlet, the quartz tube reaction zone, and the wire outlet in sequence and is fixed on the wire collecting wheel.

[0009] In this embodiment, the wire collecting machine and / or the wire releasing machine is equipped with a pre-tensioning wheel, the fibers to be processed are connected to the guide wheel mechanism through the pre-tensioning wheel, the pre-tensioning wheel is equipped with a pressure sensor, and the pressure sensor is connected to the first drive device and the second drive device through the control system. The tension of the fiber is set by the control system, and the speed of the wire releasing wheel and the wire collecting wheel is adjusted by the first drive device and the second drive device to ensure that the tension of the fiber is within the set range, which can effectively reduce the internal fiber stress, prevent the occurrence of wire breakage, reduce the probability of downtime for maintenance, and improve production efficiency.

[0010] In this embodiment, the front liquid seal box adopts catalyst liquid seal, and the rear liquid seal box adopts water seal.

[0011] In this embodiment, the top openings of the front liquid sealing box and the rear liquid sealing box are closed with a cover plate, the cover plate is provided with an opening at a position matching the inlet and outlet wire tubes, and the cover plate is provided with a groove at a position matching the fiber to be processed. The closure of the cover plate can minimize the volatilization of the solution in the liquid sealing box, save production resources, and improve utilization.

[0012] In this embodiment, the guide pulley mechanism includes a first fixed pulley, a second fixed pulley, a third fixed pulley, a fourth fixed pulley, a fifth fixed pulley and a sixth fixed pulley. The first fixed pulley is arranged below the wire inlet of the front liquid seal box, and the sixth fixed pulley is arranged below the wire outlet of the rear liquid seal box. The second fixed pulley is arranged in the quartz tube at the outlet of the wire inlet tube, and the fifth fixed pulley is arranged in the quartz tube at the inlet of the wire outlet tube. The third fixed pulley and the fourth fixed pulley are respectively arranged at the inlet and outlet ends of the reaction zone in the quartz tube, and the fiber to be processed on the wire releasing wheel bypasses the first fixed pulley, the second fixed pulley, the fourth fixed pulley, the third fixed pulley, the fifth fixed pulley and the sixth fixed pulley in turn and is connected to the wire collecting wheel.

[0013] In this embodiment, the first fixed pulley, the second fixed pulley, the third fixed pulley, the fourth fixed pulley, the fifth fixed pulley and the sixth fixed pulley are all provided with U-shaped grooves arranged along the circumferential direction and matching the size of the fibers to be processed, thereby effectively reducing the probability of fiber shedding.

[0014] In this embodiment, a plurality of U-shaped grooves may be arranged on the third and fourth fixed pulleys in the axial direction. The fiber to be processed may be wound around the third and fourth fixed pulleys for multiple times, thereby increasing the number of times the fiber to be processed travels in the reaction zone.

[0015] In summary, the present invention creates a closed environment required for continuous wire-feeding reaction through the front liquid sealing box and the rear liquid sealing box, and adjusts the atmosphere ratio, total atmosphere, reaction temperature, wire-feeding speed and other conditions by arranging the atmosphere introduction device, the tubular furnace body setting, the wire collecting machine and the wire releasing machine, so that the wire-feeding can be accurately adjusted according to the needs, ensuring the controllability, accuracy and diversity of CVD preparation, and providing technical support for continuous large-scale CVD preparation of composite fibers, carbon deposition, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the structure of the present invention.

[0017] In the attached drawings, 1. quartz tube; 11. wire inlet tube; 12. wire outlet tube; 13. first fixed pulley; 14. second fixed pulley; 15. third fixed pulley; 16. fourth fixed pulley; 17. fifth fixed pulley; 18. sixth fixed pulley; 2. atmosphere introduction device; 3. tail gas treatment device; 4. wire unwinding machine; 5. wire collecting machine; 6. front liquid sealing box; 7. rear liquid sealing box; 8. tubular furnace body; 81. heating area. DETAILED DESCRIPTION

[0018] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] In addition, the technical solutions between the various embodiments of the present invention can be combined with each other, but it must be based on the fact that ordinary technicians in the field can implement it. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0020] like Figure 1 As shown, the present invention provides a device for continuous vapor deposition wire feeding, comprising a quartz tube 1, a guide wheel mechanism, a liquid sealing box, a wire unwinding machine 4, a wire collecting machine 5, an atmosphere introduction device 2 and an exhaust gas treatment device 3, wherein the quartz tube 1 is provided with an atmosphere inlet and a wire inlet at one end, and an exhaust gas outlet and a wire outlet at the other end, the middle part of the inner cavity of the quartz tube 1 is a reaction zone, the reaction zone of the quartz tube 1 is arranged in a heating area 81 of a tubular furnace body 8, the atmosphere inlet of the quartz tube 1 is connected with the outlet of the atmosphere introduction device 2 through a pipeline, the exhaust gas outlet of the quartz tube 1 is connected with the inlet of the exhaust gas treatment device 3 through a pipeline, the two ends of the quartz tube 1 are respectively provided with a wire inlet tube 11 and a wire outlet tube 12 arranged vertically to the quartz tube 1, the wire inlet tube 11 and the wire outlet tube 12 are connected to the inner cavity of the quartz tube 1, and the wire inlet tube 11 and the wire outlet tube 12 are connected to the inner cavity of the quartz tube 1. One end is sealed and connected to the quartz tube 1, and the other end forms the wire inlet and the wire outlet. The liquid seal box includes a front liquid seal box 6 and a rear liquid seal box 7. The wire inlet of the quartz tube 1 is arranged below the liquid level of the front liquid seal box 6, and the wire outlet of the quartz tube 1 is arranged below the liquid level of the rear liquid seal box 7; the wire unwinding machine 4 is arranged on one side of the wire inlet of the quartz tube 1, and the wire collecting machine 5 is arranged on one side of the wire outlet of the quartz tube 1. The wire unwinding machine 4 includes a wire unwinding wheel driven to rotate by a first driving device, and the wire collecting machine 5 includes a wire collecting wheel driven to rotate by a second driving device. The fiber to be processed is wound on the wire unwinding wheel. The quartz tube 1, the front liquid seal box 6 and the rear liquid seal box 7 are all provided with a guide wheel mechanism. One end of the fiber to be processed passes through the wire inlet, the middle reaction zone of the quartz tube 1, and the wire outlet in sequence through the guide wheel mechanism and is fixed on the wire collecting wheel;

[0021] The guide wheel mechanism includes a first fixed pulley 13, a second fixed pulley 14, a third fixed pulley 15, a fourth fixed pulley 16, a fifth fixed pulley 17 and a sixth fixed pulley 18, wherein the first fixed pulley 13 is arranged below the inlet of the front liquid seal box 6, and the sixth fixed pulley 18 is arranged below the outlet of the rear liquid seal box 7, the second fixed pulley 14 is arranged in the quartz tube 1 at the outlet of the wire inlet tube 11, the fifth fixed pulley 17 is arranged in the quartz tube 1 at the inlet of the wire outlet tube 12, the third fixed pulley 15 and the fourth fixed pulley 16 are respectively arranged at the inlet end and the outlet end of the reaction zone in the quartz tube 1, and the fiber to be processed on the release wheel bypasses the first fixed pulley 13, the second fixed pulley 14, the fourth fixed pulley 16, the third fixed pulley 15, the fifth fixed pulley 17 and the sixth fixed pulley 18 in sequence and is connected to the collection wheel; the first fixed pulley 13, the second fixed pulley 14, the third fixed pulley 1 5. The fourth fixed pulley 16, the fifth fixed pulley 17 and the sixth fixed pulley 18 are all provided with U-shaped grooves arranged along the circumferential direction that match the size of the fiber to be processed, thereby effectively reducing the probability of wire stripping; the third fixed pulley 15 and the fourth fixed pulley 16 can be correspondingly arranged with multiple U-shaped grooves along the axial direction, and the fiber to be processed can be reciprocated around the third fixed pulley 15 and the fourth fixed pulley 16 for multiple times, thereby increasing the number of wire runs of the fiber to be processed in the reaction zone, and the number of wire runs in the reaction zone is set to n, the reaction time of the fiber to be processed is t, the main heating length in the quartz tube is l, and the moving speed of the fiber to be processed in the reaction zone is s, st=nl, the number of wire runs n can be determined according to the mechanical properties of the fiber bundle or the deposition template. When the mechanical properties of the fiber or the deposition template are better, the upper limit of the number of wire runs can be set higher during the design, and the specific number of wire runs is set according to the requirements of the actual product.

[0022] In this embodiment, the quartz tube is a quartz tube that can withstand a high temperature of at least 800°C, and the front liquid seal box 6 and the rear liquid seal box 7 are implemented by water seal or catalyst pool liquid seal. A cover plate is provided on the top opening of the front liquid seal box 6 and the rear liquid seal box 7, and the cover plate is provided with an opening at a position matching the inlet wire tube 11 and the outlet wire tube 12, and the cover plate is provided with a groove at a position matching the fiber to be processed, so that the volatilization of the solution in the liquid seal box can be reduced as much as possible, production resources can be saved, and the utilization rate can be improved.

[0023] In this embodiment, the speeds of the wire collecting machine 5 and the wire releasing machine 4 can be controlled, and the wire collecting machine 5 and the wire releasing machine 4 are equipped with pre-tensioning wheels, and the pre-tensioning wheels are equipped with pressure sensors, and the pressure sensors are connected to the first driving device and the second driving device through the control system; the tensioning force of the fiber is set by the control system, and the speeds of the wire releasing wheel and the wire collecting wheel are adjusted by the first driving device and the second driving device to ensure that the tensioning force of the fiber is within the set range, which can effectively reduce the internal fiber stress, prevent the occurrence of wire breakage, reduce the probability of shutdown for maintenance, and improve production efficiency.

[0024] In this embodiment, the atmosphere introduction device 2 is provided with a gas flow control system, which can adjust the component proportions, entry time and other operation details of the multiple atmospheres entering the quartz tube 1, and can be adjusted as needed. The tail gas treatment device 3 is provided with an exhaust device to discharge the reaction gas in the quartz tube 1.

[0025] With this device, after assembling the entire equipment system, the fiber is connected to the wire collecting machine 5 and the wire releasing machine 4 through the rollers in the system. By changing the atmosphere ratio, atmosphere type, reaction temperature, catalyst type, fiber type and other conditions, it is possible to produce carbon nanotube-modified fibers with specific morphology, which have improved dielectric and mechanical properties and have good application prospects in the fields of absorbing materials, composite material reinforcement, etc. The overall equipment has a simple structure, is easy to operate, and can achieve continuous CVD production.

[0026] Embodiment 1:

[0027] Ferrocene was weighed with an electronic scale and added to xylene. Ultrasonication was performed for 30 minutes to prepare a ferrocene / xylene catalyst with a concentration of 0.05 g / ml. The ferrocene / xylene catalyst was added to the front liquid seal box as the catalyst liquid seal in the front liquid seal box. Deionized water was added to the rear liquid seal box as the liquid seal of the rear liquid seal box to ensure that the reaction gas in the quartz tube eventually led to the exhaust gas treatment device.

[0028] First, argon gas is introduced into the quartz tube for 30 minutes at a flow rate of 800sccm, and the air in the reaction environment is exhausted as much as possible. The tubular furnace is controlled to execute the heating program, and argon gas is continuously introduced. When the temperature of the heating area of ​​the tubular furnace reaches 500°C, hydrogen gas is introduced into the quartz tube at a flow rate of 80-180sccm. When the temperature of the heating area of ​​the tubular furnace reaches 740°C and the temperature is stable for 5 minutes, the temperature of the heating area of ​​the tubular furnace is maintained, acetylene is introduced into the quartz tube at a flow rate of 25sccm, and the wire collecting machine and wire releasing machine are started to start wire drawing. The wire drawing rate is 0.05m / min, and the time for silicon carbide to grow carbon nanotubes in the reaction environment is 7min. Silicon carbide fibers modified with carbon nanotubes can be obtained, and their dielectric and mechanical properties are improved.

[0029] The above are only preferred embodiments of the present invention, and are not intended to limit the patent scope of the present invention. All equivalent structural changes made using the contents of the present invention's specification and drawings, or directly / indirectly applied in other related technical fields, are included in the patent protection scope of the present invention.

Claims

1. A device for continuous vapor deposition wire feeding, characterized in that: The invention comprises a quartz tube (1), a guide wheel mechanism, a liquid sealing box, an atmosphere introduction device (2) and an exhaust gas treatment device (3); one end of the quartz tube (1) is provided with an atmosphere inlet and a wire inlet, and the other end is provided with an exhaust gas outlet and a wire outlet; the middle part of the inner cavity of the quartz tube (1) is a reaction zone; the reaction zone of the quartz tube (1) is arranged in a heating area (81) of a tubular furnace body (8); the atmosphere inlet of the quartz tube (1) is connected to the outlet of the atmosphere introduction device (2) through a pipeline; The tail gas outlet of the quartz tube (1) is connected to the inlet of the tail gas treatment device (3) through a pipeline; the liquid seal box comprises a front liquid seal box (6) and a rear liquid seal box (7); the wire inlet of the quartz tube (1) is arranged below the liquid level of the front liquid seal box (6), and the wire outlet of the quartz tube (1) is arranged below the liquid level of the rear liquid seal box (7); the guide wheel mechanism guides the fiber to be treated from the wire inlet of the quartz tube, passes through the reaction zone in the middle of the inner cavity of the quartz tube, and leads out from the wire outlet; The two ends of the quartz tube (1) are respectively provided with a wire inlet tube (11) and a wire outlet tube (12) arranged perpendicularly to the quartz tube (1); the wire inlet tube (11) and the wire outlet tube (12) are communicated with the inner cavity of the quartz tube (1); one end of the wire inlet tube (11) and the wire outlet tube (12) are sealed with the quartz tube (1), and the other end forms the wire inlet port and the wire outlet port; the wire inlet tube (11) and the wire outlet tube (12) at the two ends of the quartz tube (1) are respectively arranged below the liquid level in the front liquid seal box (6) and the rear liquid seal box (7).

2. The device for continuous vapor deposition wire feeding as claimed in claim 1, characterized in that: The invention also comprises a wire unwinding machine (4) and a wire collecting machine (5), wherein the wire unwinding machine (4) is arranged on one side of a wire inlet of the quartz tube (1), and the wire collecting machine (5) is arranged on one side of a wire outlet of the quartz tube (1), wherein the wire unwinding machine (4) comprises a wire unwinding wheel driven to rotate by a first driving device, and the wire collecting machine (5) comprises a wire collecting wheel driven to rotate by a second driving device, wherein fibers to be processed are wound around the wire unwinding wheel, wherein one end of the fibers to be processed is fixed to the wire unwinding wheel, and the other end passes through the wire inlet, the quartz tube reaction zone, and the wire outlet in sequence and is fixed to the wire collecting wheel.

3. The device for continuous vapor deposition wire feeding as claimed in claim 2, characterized in that: The wire collecting machine (5) and / or the wire releasing machine (4) are equipped with a pre-tensioning wheel, the fibers to be processed are connected to the guide wheel mechanism via the pre-tensioning wheel, the pre-tensioning wheel is equipped with a pressure sensor, and the pressure sensor is connected to the first drive device and the second drive device via a control system.

4. The device for continuous vapor deposition wire feeding as claimed in claim 1, characterized in that: The front liquid seal box (6) adopts catalyst liquid seal, and the rear liquid seal box (7) adopts water seal.

5. The device for continuous vapor deposition wire feeding as claimed in claim 4, characterized in that: The top openings of the front liquid sealing box (6) and the rear liquid sealing box (7) are closed by a cover plate, the cover plate is provided with an opening at a position matching the inlet wire tube (11) and the outlet wire tube (12), and the cover plate is provided with a groove at a position matching the fiber to be processed.

6. The device for continuous vapor deposition wire feeding as claimed in claim 2, characterized in that: The guide wheel mechanism comprises a first fixed pulley (13), a second fixed pulley (14), a third fixed pulley (15), a fourth fixed pulley (16), a fifth fixed pulley (17) and a sixth fixed pulley (18); the first fixed pulley (13) is arranged below the wire inlet of the front liquid seal box (6); the sixth fixed pulley (18) is arranged below the wire outlet of the rear liquid seal box (7); the second fixed pulley (14) is arranged inside the quartz tube (1) at the outlet of the wire inlet tube (11); The fifth fixed pulley (17) is arranged in the quartz tube (1) at the inlet of the wire outlet tube (12); the third fixed pulley (15) and the fourth fixed pulley (16) are arranged at the inlet end and the outlet end of the reaction zone in the quartz tube (1), respectively; the fiber to be processed on the unwinding wheel sequentially passes around the first fixed pulley (13), the second fixed pulley (14), the fourth fixed pulley (16), the third fixed pulley (15), the fifth fixed pulley (17) and the sixth fixed pulley (18) to be connected to the collecting wheel.

7. The device for continuous vapor deposition wire feeding as claimed in claim 6, characterized in that: The first fixed pulley (13), the second fixed pulley (14), the third fixed pulley (15), the fourth fixed pulley (16), the fifth fixed pulley (17) and the sixth fixed pulley (18) are all provided with U-shaped grooves arranged along the circumferential direction and matching the size of the fibers to be processed.

8. The device for continuous vapor deposition wire feeding as claimed in claim 7, characterized in that: A plurality of U-shaped grooves are correspondingly arranged on the third fixed pulley (15) and the fourth fixed pulley (16) along the axial direction.

Images