A chemical vapor deposition reaction device suitable for uniform and continuous large-area preparation of segmented membrane materials
Through the design of a motor-controlled local pushing device and a gas uniform phase distributor, the problems of airtightness and uniformity of chemical vapor deposition reaction equipment in the preparation of segmented thin film materials are solved, efficient and continuous material preparation is achieved, and production efficiency and material quality are improved.
Patent Information
- Application Number
- CN202311165463.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-08
- Publication Date
- 2025-09-19
- Estimated Expiration
- 2043-09-08
AI Technical Summary
Existing chemical vapor deposition reaction equipment has problems such as insufficient airtightness, unstable transmission, low production efficiency, and poor material uniformity in the uniform, continuous, efficient, and high-quality preparation of segmented thin film materials. In particular, it is difficult to ensure atmosphere uniformity and material integrity in high-temperature environments.
The motor-controlled local push device is designed with coaxially aligned material transfer guides, loading fixtures and buffer bins. Combined with a gas phase distributor directly reaching the center of the reaction zone and protective gas at the air inlet end, a gas barrier is formed to ensure accurate material transportation and continuous preparation in a high-temperature environment, avoiding airtightness problems. Efficient transportation is achieved through a complete vacuum system and sealing structure.
The ultra-high airtightness continuous preparation of segmented membrane materials is achieved, ensuring that the material experiences the same growth environment at each position, improving material quality and production efficiency, reducing production costs, and breaking through the limitations of material size, especially length.
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Figure CN117107218B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of chemical vapor deposition reaction equipment, in particular to a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials. Background Art
[0002] Chemical vapor deposition (CVD) is one of the main methods for the controllable preparation of large-scale materials, and is particularly suitable for depositing layered thin film materials on various substrates. Compared with traditional preparation methods such as chemical synthesis or liquid phase exfoliation, the chemical vapor deposition process has the following advantages: (1) it can achieve atomic-level controllable assembly and precisely control the number of material layers, thickness, area and other indicators; (2) the preparation cycle is short, and the deposition process can be completed within seconds or minutes; (3) because the chemical vapor deposition process is generally carried out under specific substrates (especially catalytically active metal substrates) and temperatures and in a protective or reducing atmosphere with good airtightness, the prepared materials are flat and have high crystalline quality. Therefore, the CVD process has broad application prospects in the field of new material preparation.
[0003] However, the CVD process still faces many problems in the preparation of materials, especially the uniform, continuous, efficient and high-quality preparation of segmented thin film materials, which seriously hinders the further application and development of this technology: (1) Chemical vapor deposition reactions generally involve flammable and explosive gases such as hydrogen, methane, and ammonia, and the reaction is generally completed at a relatively high temperature. If the system is not airtight, it will not only cause great safety hazards, but also seriously affect the quality of the prepared materials due to the infiltration of oxygen in the air. For airtightness considerations, general chemical vapor deposition devices can only adopt a reaction method in which the sample is heated and cooled with the furnace, which is very time-consuming and energy-consuming. (2) Although some CVD equipment is also equipped with a push-pull rod that runs through the reaction zone to send the sample into or out of the high-temperature reaction zone, these devices can only rely on manual control of the push-pull rod to feed and take out the material, and the process is random and uncontrollable; or the push-pull rod and other parts use simple sealing rings or sealed bearings to be directly connected to the external drive motor, and the airtightness of the system is difficult to be effectively guaranteed under a dynamic sealing environment. At the same time, an overly long push-pull rod not only takes up a lot of space, but will inevitably deform due to gravity, especially when the push operation is completed and the rod is withdrawn from the high-temperature zone, which will seriously affect the airtightness of the entire system. (3) Although the use of push-pull rods avoids frequent temperature increases and decreases in the heating furnace body and saves some time, each time the reaction furnace chamber is opened for loading and unloading, more than two cycles of evacuation / emptying of reaction gas-filling of protective gas are still required. Continuous loading and collection of samples cannot be achieved, and production efficiency is still low. Although some equipment is equipped with simple feeding and receiving devices, due to the lack of a buffer bin and an automatically controlled buffer bin door design, it can only achieve batch feeding and collection, and cannot truly achieve an uninterrupted, continuous, and automated reaction process. (4) Although some growth equipment uses a conveyor crawler structure that runs through the entire furnace tube cavity and is directly driven by an external motor (which also faces the airtightness problem described in Article 2) or indirectly in order to achieve continuous sample transmission, it is not possible to achieve continuous transmission of samples. However, on the one hand, because the conveyor belt needs to pass through the high temperature zone (the temperature can reach thousands of degrees Celsius) and the reaction atmosphere, the conveyor belt made of most materials cannot meet the requirements of strength, thermal stability and service life at the same time; on the other hand, the belt that runs through the entire furnace tube cavity undergoes drastic temperature changes during the transmission process (the temperature difference between the normal temperature zone and the high temperature zone can reach thousands of degrees Celsius). The significant deformation caused by thermal expansion and contraction will inevitably lead to jamming and transmission failure in its actual operation, and it is impossible to ensure the stability and controllability of the transmission process; at the same time, the double-layer track structure of the circular transmission will greatly occupy the space in the furnace tube, limit the size of the sample accommodated (especially in the width direction), and cause significant disturbances to the temperature and air flow in the reaction zone, seriously affecting the uniformity and quality of the prepared material. (5) For some flexible thin film materials prepared on high-temperature resistant flexible substrates, although some inventions have proposed setting a discharge shaft and a receiving shaft on both sides of the equipment (such as direct drive by an external motor-driven seal, which still faces the problem of airtightness), the idea of using the growth substrate (such as copper foil) itself as a transmission device.However, on the one hand, this method is only suitable for growing flexible films on large-scale continuous-length high-temperature resistant flexible substrates, and is not suitable for segmented, block, and rigid samples. On the other hand, during the reaction process, due to the large tensile stress on the substrate material under high temperature, cracks and other defects are easily generated in the growing material, which seriously affects the quality of the prepared material. (6) For segmented substrates, especially thin substrates, if the substrate itself is pushed directly, it will not only cause the sample to be subjected to large extrusion stress, but also easily cause the substrate to be too thin during the mutual transmission process, causing the transmission process to jam or fail. (7) On the other hand, if the substrate material is simply used to transmit and transfer each other in the reaction zone, when the amount of segmented substrate material left is small, it cannot be guaranteed that each section of raw material can fully pass through the reaction zone and reach the finished product area for collection. (8) Due to the limitation of the furnace body size, especially the length of the constant temperature zone, the size and especially the length of the sample prepared in a single furnace are limited. Generally, the atmosphere required for chemical vapor deposition reaction is a mixture of several gases, and the air inlet is a single opening set on the air inlet end flange. During the process of the reaction gas diffusing over a long distance to the constant temperature zone of the open structure furnace, due to the different gas densities and proportions, under the influence of gravity and gas flow rate, the atmosphere environment in different positions of the CVD reaction zone, such as the front and back, and the top and bottom, is significantly different, making it difficult to ensure the uniformity of the prepared materials. (9) On the one hand, the general support boat will cause significant disturbances to the temperature and atmosphere of the reaction zone because it enters and exits the high-temperature reaction zone along with the sample. On the other hand, it will also affect the growth of the material due to blocking the airflow and the large contact area with the substrate, especially the growth on the lower surface of the substrate, which is not conducive to the efficient and high-quality preparation of materials. Summary of the Invention
[0004] The purpose of the present invention is to provide a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials, which realizes the precise transmission and continuous preparation of materials under ultra-high airtightness, ensures that the segmented membrane material substrate experiences the same growth environment at each position during the continuous preparation process, and both the upper and lower surfaces of the material can participate in the reaction to grow thin films. The reaction process is uniform and efficient and greatly breaks through the material size, especially the length limitation.
[0005] The technical solution of the present invention is:
[0006] A chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials. The equipment consists of a gas supply system, a raw material area, a reaction area, a finished product area, and an exhaust and vacuum system. The specific structure is as follows:
[0007] The raw material bin in the raw material area is connected to the feed end of the reactor tube in the reaction area, and the finished product bin in the finished product area is connected to the discharge end of the reactor tube in the reaction area; the gas supply system is connected to the protective gas pipeline interface in the raw material area through the first protective gas pipeline, the gas supply system is connected to the protective gas pipeline interface in the finished product area through the second protective gas pipeline and the third protective gas pipeline, and the gas supply system is connected to the reaction gas pipeline interface in the finished product area through the reaction gas pipeline; the vacuum pump of the tail gas and vacuum system is connected to the vacuum pipeline interface in the raw material area through the first vacuum pipeline and the second vacuum pipeline respectively, and the vacuum pump of the tail gas and vacuum system is connected to the vacuum pipeline interface in the finished product area through the third vacuum pipeline; the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface in the raw material area through the first tail gas pipeline and the second tail gas pipeline after passing through the second check valve, the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface in the finished product area through the third tail gas pipeline after passing through the second check valve, and the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface of the vacuum system through the fourth tail gas pipeline after passing through the second check valve;
[0008] A raw material buffer bin is provided above the raw material bin in the raw material area, and a finished product buffer bin is provided below the finished product bin in the finished product area; the push rail in the raw material area is coaxially aligned with the feed guide rail in the reaction area, and the feed guide rail is coaxially placed in the reaction furnace tube in the reaction area.
[0009] The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials, the gas supply system includes a gas source, a gas circuit valve, a mass flow controller, a gas mixer and a gas pipeline, and the specific structure is as follows: the gas source is two or more gases including reaction gas and protective gas, the gas pipeline includes a reaction gas pipeline and a protective gas pipeline, the gas source of the reaction gas is connected to the reaction gas pipeline interface of the finished product area through the gas circuit valve, the mass flow controller, the gas mixer, the reaction gas pipeline, and the reaction gas pipeline interface, the gas source of the protective gas is connected to the protective gas pipeline interface of the raw material area or the finished product area through the gas circuit valve, the mass flow controller, the protective gas pipeline, the reaction gas pipeline transports reaction gas to the equipment, and the protective gas pipeline transports protective gas to the equipment; the gas mixer mixes two or more gases at the same time to prevent gas stratification in the pipeline; the gas mixing mode of the gas mixer is static mixing or dynamic mixing, and its internal structure is SV type, K type, SX type, SH type, SL type, SY type or SD type.
[0010] The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials is described. The raw material bin in the raw material area is installed on the bracket, and a horizontal raw material bin outer door is provided at the opening of the upper flange. A horizontal raw material bin inner door is provided below the raw material bin outer door in the inner cavity of the raw material bin. The chamber formed between the raw material bin outer door and the raw material bin inner door is a raw material bin buffer bin. A pushing rail is provided at the bottom of the inner cavity of the raw material bin. The outer wall of the pushing rail is semi-cylindrical and follows the shape of the inner wall of the raw material bin. The inner wall of the pushing rail is symmetrically provided with a guide rail. The upper part of the guide rail of the pushing rail corresponds to the pushing plate of the local pushing device. A raw material end sealing flange is installed on the side of the raw material bin close to the local pushing device, and a water-cooled sealing flange is provided on the other side of the raw material bin at the connection between the raw material bin and the feed end of the reaction furnace tube in the reaction zone.
[0011] The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials is connected to a local pushing device at the tail end of the raw material warehouse. The specific structure of the local pushing device is as follows:
[0012] The sealing flange at the push end corresponds to the sealing flange at the raw material end and is sealed and fixed to the tail end of the raw material bin by screws. A sleeve is coaxially integrated on one side of the sealing flange at the push end. One end of the transmission rod passes through the sealing flange at the raw material end and is sealed in the sleeve on one side of the sealing flange at the push end. The other end of the transmission rod is connected to the horizontal push plate through a transmission connector. The push plate is in sliding cooperation with the push rail in the inner cavity of the raw material bin.
[0013] The sleeve is equipped with a linear slide module connecting sleeve, which is connected to the slider on the linear slide module through a connecting plate. The linear slide module connecting sleeve slides back and forth on the linear slide module through the slider, further driving the transmission rod, transmission connector, and push plate to move;
[0014] The transmission module magnet and the transmission module linear bearing are coaxially arranged between the inner side of the linear slide module connecting sleeve and the sleeve, and magnetic transmission module limits are set at both ends of the transmission module magnet and the transmission module linear bearing; the driven module magnet and the driven module linear bearing are coaxially fixed between the outer side of one end of the transmission rod extending into the sleeve and the sleeve, and magnetic driven module limits are set at both ends of the driven module magnet and the driven module linear bearing.
[0015] The chemical vapor deposition reaction equipment suitable for the uniform and continuous large-area preparation of segmented membrane materials, the outer door of the raw material bin and the inner door of the raw material bin are compressed by fasteners or pressurization to form metal gaskets, narrow face seals, self-tightening seals, flat gasket seals, Kazari seals, double cone seals, Wood seals, C-type seals or hollow metal O-ring seals; the inner door of the raw material bin is pressurized and sealed and opened and closed by planar movement by one of a pull-type electromagnet, a push-type electromagnet or a pneumatic telescope.
[0016] The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials is sealed between the upper flange of the raw material bin and the outer door of the raw material bin by an O-ring gasket, and fastening screw holes are symmetrically opened on the end face of the upper flange of the raw material bin. Fasteners pass through the outer door of the raw material bin and the upper flange of the raw material bin and are installed in the fastening screw holes, so that the outer door of the raw material bin and the upper flange of the raw material bin are sealed and connected;
[0017] The raw material warehouse is installed in the form of a plug-in plate in the inner cavity of the raw material warehouse below the outer door of the raw material warehouse. The lower ends of the inner door of the raw material warehouse are sealed with the side walls of the inner cavity of the raw material warehouse by square sealing gaskets. The upper ends of the inner door of the raw material warehouse are symmetrically arranged with longitudinal pneumatic expanders. The pneumatic expanders are connected to the pneumatic expander air source pipeline, and the lifting of the pneumatic expander is controlled by the pneumatic expander air source pipeline; the outer end of the inner door of the raw material warehouse is provided with a screw, and the inner door of the raw material warehouse is connected to the spiral O-type sealing nut through the screw, and the opening or closing of the inner door of the raw material warehouse is controlled by the spiral O-type sealing nut.
[0018] The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials is characterized in that the materials to be reacted are directly placed on the push rail, or the materials to be reacted are placed on the push rail after being clamped by a material carrier, or a material transfer plate is placed on the push rail;
[0019] The loading fixture includes a loading fixture limit bolt, an upper limit sleeve of the loading fixture, and a lower limit sleeve of the loading fixture. The upper limit sleeve of the loading fixture and the lower limit sleeve of the loading fixture are rectangular frame structures arranged relatively up and down. The material to be reacted is located between the upper limit sleeve of the loading fixture and the lower limit sleeve of the loading fixture. The upper limit sleeve of the loading fixture and the lower limit sleeve of the loading fixture are connected and fixed by the loading fixture limit bolt; the material transfer plate is arranged on one side of the material to be reacted, and the material transfer plate is evenly and densely arranged with air holes.
[0020] The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials, the reaction zone includes a tubular heating furnace, a reaction furnace tube, a feed guide rail and a gas uniform phase distributor, and the specific structure is as follows: the reaction furnace tube is horizontally arranged in the tubular heating furnace, the feed guide rail is arranged in the lower half of the inner cavity of the reaction furnace tube, the outer wall of the feed guide rail is semi-cylindrical and follows the shape of the inner wall of the reaction furnace tube, and a gas uniform phase distributor is installed at the upper opening of the feed guide rail. The gas uniform phase distributor is an open groove structure, and an air outlet plate is embedded in the upper opening. The air outlet plate surface is densely arranged with air outlet holes of the gas uniform phase distributor. The number of the air outlet holes of the gas uniform phase distributor gradually becomes denser along the air inlet direction, and the aperture of the air outlet holes of the gas uniform phase distributor gradually becomes larger from the central axis on both sides. The gas uniform phase distributor is connected to the reaction gas pipeline through the gas uniform phase distributor air inlet interface opened on its side;
[0021] The inner cavity of the gas uniform phase distributor is a gas uniform phase distributor gas uniform cavity. The gas uniform phase distributor gas uniform cavity is provided with an air inlet channel connected to the air inlet interface of the gas uniform phase distributor. Air dividing cavities are symmetrically arranged on both sides of the air inlet channel. The air dividing cavities are open groove structures. A vent is provided on the side of the air dividing cavities corresponding to the air inlet channel. The air inlet channel is connected to the air dividing cavities through the vent. The vents are arranged according to the rule of gradually becoming larger along the air inlet direction.
[0022] The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials is described, and the finished product bin in the finished product area is installed on a bracket, a horizontal finished product bin outer door is provided at the flange opening at the lower end of the finished product bin, a horizontal finished product bin inner door is provided above the finished product bin outer door in the inner cavity of the finished product bin, and the chamber formed between the finished product bin outer door and the finished product bin inner door is the finished product bin buffer bin, and a water-cooled sealing flange is provided at the connection between the finished product bin and the discharge end of the reaction furnace pipe in the reaction zone; the air supply system is connected to the reaction gas pipeline interface at the feed end of the finished product bin through the reaction gas pipeline, is connected to the second protective gas pipeline at the tail end of the finished product bin, and is connected to the third protective gas pipeline on the side of the finished product bin buffer bin;
[0023] The lower flange of the finished product bin and the outer door of the finished product bin are sealed by an O-ring gasket, and fastening screw holes are symmetrically opened on the end face of the lower flange of the finished product bin. Fasteners pass through the outer door of the finished product bin and the lower flange of the finished product bin and are installed in the fastening screw holes, so that the outer door of the finished product bin and the lower flange of the finished product bin are sealed and connected;
[0024] The inner door of the finished product warehouse is installed in the inner cavity of the finished product warehouse above the outer door of the finished product warehouse in the form of a plug-in plate. The upper two ends of the inner door of the finished product warehouse are sealed with the side walls of the inner cavity of the finished product warehouse by square sealing gaskets. The lower two ends of the inner door of the finished product warehouse are symmetrically provided with longitudinal pneumatic expanders, which are connected to the pneumatic expander air source pipeline, and the lifting and lowering of the pneumatic expander are controlled by the pneumatic expander air source pipeline; the outer end of the inner door of the finished product warehouse is provided with a screw, and the inner door of the finished product warehouse is connected to the spiral O-type sealing nut through the screw, and the opening or closing of the inner door of the finished product warehouse is controlled by the spiral O-type sealing nut.
[0025] The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials, the tail gas and vacuum system includes a tail gas system and a vacuum system, the tail gas system is provided with a tail gas treatment device, a second check valve and a tail gas pipeline, and the vacuum system is provided with a vacuum pump, a first check valve and a vacuum pipeline;
[0026] The tail gas treatment device is connected to the second check valve and is closely connected to the equipment tail gas pipeline through a pipeline. When it is opened, it maintains the entire equipment cavity or the raw material warehouse / raw material buffer warehouse, finished product warehouse / finished product buffer warehouse at normal pressure. The tail gas treatment device is one or a combination of two or more of an absorption liquid container, a desiccant container, and an activated carbon container. A solution for neutralizing or absorbing harmful tail gas is added to the absorption liquid container, a desiccant is added to the desiccant container, and activated carbon is added to the activated carbon container.
[0027] The vacuum pump is connected to the first check valve and is tightly connected to the equipment vacuum pipeline through a pipeline. When turned on, it realizes a negative pressure growth environment of the equipment or absorbs the air or reaction gas in the entire sealed cavity or raw material buffer bin. The vacuum pump is a dry screw vacuum pump, a water ring pump, a reciprocating pump, a sliding valve pump, a rotary vane pump, a Roots pump or a diffusion pump.
[0028] The principle of the present invention is:
[0029] The present invention realizes the precise pushing and continuous preparation of materials under ultra-high air tightness through the motor-controlled compartment induction-driven local pushing device in conjunction with the pushing support rail and the adjacent coaxially aligned material transfer guide rail, loading fixture, material transfer plate and raw material bin and finished product bin with buffer bin; the gas barrier formed by the gas uniform distributor directly reaching the center of the reaction zone and the continuously supplied inlet end protective gas ensures that the segmented membrane material substrate experiences the same growth environment at each position during the continuous preparation process, and both the upper and lower surfaces of the material can participate in the reaction to grow the thin film. The reaction process is uniform and efficient and has greatly broken through the material size, especially the length limitation. It has the characteristics of simplicity, high efficiency, flexible combination and wide range of applications.
[0030] The advantages and beneficial effects of the present invention are:
[0031] 1. The present invention proposes a continuous and precise pushing device indirectly driven by external induction controlled by a motor, in conjunction with a pushing rail and a material feeding guide rail coaxially aligned with it, a loading fixture / transfer plate, and a raw material bin and a finished product bin with a buffer bin, thereby realizing precise pushing and continuous preparation of materials under ultra-high airtightness; at the same time, the gas uniform distributor directly reaching the center of the reaction zone and the gas barrier effect generated by the continuous supply of protective gas separately arranged at the air inlet end jointly ensure that each position of the continuously growing base material can experience the same growth environment in turn, thereby significantly breaking through the limitations of the equipment volume, the length of the constant temperature zone, and the changes in the atmosphere at different positions on the size of the prepared materials, especially the length of the materials.
[0032] 2. This invention utilizes a motor to control an externally coupled magnet compartment induction to indirectly drive a localized push mechanism within the device, achieving controllable transmission. This avoids the need for various dynamic sealing interfaces and ensures the device's extremely high airtightness. Furthermore, because this invention is equipped with a comprehensive vacuum system, it can accommodate specialized reactions requiring negative pressure environments.
[0033] 3. The present invention proposes to control the pushing device through a programmable motor to ensure the precise control of the feeding, reaction and receiving processes.
[0034] 4. This invention proposes replacing through-type push-pull rods or tracks with a localized pusher mechanism, a pusher support rail, and a material transfer guide positioned below it, sealed and stationary, to coordinate the material loading fixture / raw material / transfer plate. This solution not only avoids the challenges to equipment stability and airtightness posed by the pusher mechanism entering the high-temperature zone, but also overcomes the limitations imposed on the pusher mechanism's material quality by the high temperatures and complex atmosphere of the reaction zone. Furthermore, because the material transfer guide rail remains stationary during operation, it avoids temperature and atmosphere disturbances caused by the pusher mechanism or carrier boat entering the high-temperature reaction zone during the reaction.
[0035] 5. The present invention proposes that the material feeding guide rail has a full-length open structure to prevent blocking the airflow and causing disturbances. In addition, its edge is serrated to achieve the purpose of reducing its contact area with the substrate and ensuring air permeability.
[0036] 6. The present invention proposes a simple method of setting appropriate gaps among the local pushing device, the pushing rail and the bottom edge of the raw material bin. On the one hand, it ensures that the pushing process is one-way, and on the other hand, it ensures that only one piece of raw material is delivered each time during the pushing process.
[0037] 7. The present invention proposes to set up a gas homogeneous distributor directly reaching the center of the reaction zone to ensure that the reaction gas will not be stratified due to diffusion before reaching the center of the reaction zone, and will be more uniform under the action of the homogeneous pores.
[0038] 8. The present invention proposes to utilize the guiding effect of the gas uniform distributor and the gas barrier effect generated by the continuous supply of protective gas separately set at the gas inlet end to promote the concentration of the reaction atmosphere in the center of the reaction zone, ensuring that the preparation process is more uniform and efficient.
[0039] 9. The present invention proposes that a uniform gas chamber is provided inside the gas phase distributor, and the uniform gas chamber is not a simple single chamber structure. A plurality of interconnected gas separation chambers are provided in the uniform gas chamber, and the air vents of the chambers are arranged in a rule that gradually increases in size along the air inlet direction. A plurality of air outlet holes are provided on the surface of the gas phase distributor, and the air outlet holes are arranged in a rule that gradually increases in number along the air inlet direction and gradually increases in size from the central axis to both sides. These specific structural designs can fully ensure that the reaction gas forms a uniform atmosphere environment in the constant temperature section in the center of the reaction zone after passing through the gas phase distributor, and the prepared material is uniform at all positions.
[0040] 10. The present invention proposes a material loading fixture design to avoid the situation where the sample is subjected to greater extrusion stress due to directly pushing the substrate itself for thinner substrate materials, and the transmission process is prevented from being stuck or failing due to the substrate being too thin and warping during the mutual transmission process.
[0041] 11. The present invention proposes a material transfer plate design to avoid the problem that when the original amount or remaining amount of the base material is small, the equipment simply uses the base material to transmit and transfer each other in the reaction zone and cannot ensure that each section of raw material can fully pass through the reaction zone and reach the finished product area for collection.
[0042] 12. The present invention is simple, efficient, flexible, and widely applicable. Through the aforementioned series of improvements and innovations, the present invention's equipment provides a continuous, uniform, and efficient growth environment for the production of segmented thin film materials. This significantly improves material quality and production efficiency, while significantly reducing production costs. BRIEF DESCRIPTION OF THE DRAWINGS
[0043] Figure 1 . Schematic diagram of the overall structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0044] Figure 2 . Schematic diagram of the pusher end of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0045] Figure 3 . Schematic diagram of a pushing device of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0046] Figure 4 .Cross-sectional view of a pushing device of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0047] Figure 5 . Exploded view of a pushing device of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0048] Figure 6 .Schematic diagram of the raw material end structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0049] Figure 7 A cross-sectional view of the raw material bin at the raw material end of a chemical vapor deposition reaction device suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0050] Figure 8 . A schematic structural diagram of a raw material end push-support rail of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0051] Figure 9 . Schematic diagram of the reaction zone structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0052] Figure 10. Schematic diagram of the reaction zone material transfer guide structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0053] Figure 11 .Top view of a gas homogeneous distributor for a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0054] Figure 12 . Exploded view of a gas homogeneous distributor of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0055] Figure 13 .Schematic diagram of the finished product area structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0056] Figure 14 A cross-sectional view of the finished product area and finished product bin of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0057] Figure 15 . Schematic diagram of the material loading fixture structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0058] Figure 16 .Schematic diagram of the vacuum system structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0059] Figure 17 .Schematic diagram of the exhaust system structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0060] Figure 18 .Schematic diagram of the material transfer plate structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0061] Figure 19 .Schematic diagram of the gas supply system structure of a chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials.
[0062] In the figure, A is the air supply system; B is the raw material area; C is the reaction area; D is the finished product area; E is the exhaust and vacuum system; 1 is the linear slide module; 2 is the stable base of the linear slide module; 3 is the sealing flange of the push end; 4 is the connecting sleeve of the linear slide module; 5 is the limit of the magnetic transmission module; 6 is the limit of the magnetic driven module; 7 is the magnet of the transmission module; 8 is the magnet of the driven module; 9 is the linear bearing of the driven module; 10 is the linear bearing of the transmission module; 11 is the transmission rod; 12 is the transmission connector; 13 is the push plate; 14 is the sealing flange of the raw material end ; 15 Raw material bin; 16 Push rail; 17 Bracket; 18 First exhaust gas pipeline; 19 First vacuum pipeline; 20 Second exhaust gas pipeline; 21 Second vacuum pipeline; 22 First protective gas pipeline; 23 O-type sealing gasket; 24 Square sealing gasket; 25 Pneumatic expansion joint; 26 Pneumatic expansion joint gas source pipeline; 27 Fastening screw hole; 28 Raw material bin inner door; 29 Sealing nut; 30 Raw material bin outer door; 31 Reaction furnace tube; 32 Feeding guide rail; 33 Gas phase distributor; 34 Reaction Gas pipeline; 35 gas phase distributor outlet; 36 gas phase distributor inlet interface; 37 finished product warehouse; 38 second protective gas pipeline; 39 third protective gas pipeline; 40 third tail gas pipeline; 41 third vacuum pipeline; 42 finished product warehouse lower end flange; 43 finished product warehouse outer door; 44 finished product warehouse inner door; 45 loading fixture limit bolt; 46 loading fixture upper limit sleeve; 47 loading fixture lower limit sleeve; 48 material to be reacted; 49 vacuum pump; 50 first check valve; 51 fourth tail Gas pipeline; 52 second check valve; 53 material transfer plate; 54 mass flow controller; 55 gas circuit valve; 56 gas mixer; 57 tubular heating furnace; 58 absorption liquid container; 59 desiccant container; 60 activated carbon container; 61 raw material warehouse buffer bin; 62 finished product warehouse buffer bin; 63 gas uniform distributor uniform gas cavity; 64 water-cooled sealing flange; 65 guide rail; 66 sleeve; 67 connecting plate; 68 slider; 69 gas outlet plate; 70 air inlet channel; 71 air vent; 72 gas distribution cavity. DETAILED DESCRIPTION
[0063] like Figures 1-19 As shown, the chemical vapor deposition reaction equipment of the present invention, which is suitable for uniform and continuous large-area preparation of segmented membrane materials, is composed of a gas supply system A, a raw material area B, a reaction area C, a finished product area D, and an exhaust gas and vacuum system E. The specific structure is as follows:
[0064] The raw material bin 15 of the raw material area B is connected to the feed end of the reaction furnace pipe 31 of the reaction area C, and the finished product bin 37 of the finished product area D is connected to the discharge end of the reaction furnace pipe 31 of the reaction area C; the gas supply system A is connected to the protective gas pipeline interface of the raw material area B through the first protective gas pipeline 22, and the gas supply system A is connected to the protective gas pipeline interface of the finished product area D through the second protective gas pipeline 38 and the third protective gas pipeline 39. The gas supply system A is connected to the reaction gas pipeline interface of the finished product area D through the reaction gas pipeline 34; the vacuum pump 49 of the tail gas and vacuum system E passes through the first check valve 50 and is connected to the vacuum pump 49 of the raw material area B through the first vacuum pipeline 19 and the second vacuum pipeline 21 respectively. The exhaust gas and vacuum system E are connected to the vacuum pipeline interface of the finished product area D through the third vacuum pipeline 41 after passing through the first check valve 50; the exhaust gas and vacuum system E's exhaust system is connected to the exhaust pipeline interface of the raw material area B through the first exhaust pipeline 18 and the second exhaust pipeline 20 after passing through the second check valve 52, the exhaust gas and vacuum system E's exhaust system is connected to the exhaust pipeline interface of the finished product area D through the third exhaust pipeline 40 after passing through the second check valve 52, and the exhaust gas and vacuum system E's exhaust system is connected to the exhaust pipeline interface of the vacuum system through the fourth exhaust pipeline 51 after passing through the second check valve 52.
[0065] A raw material buffer bin 61 is located above the raw material bin 15 in raw material zone B, and a finished product buffer bin 62 is located below the finished product bin 37 in finished product zone D. The push rail 16 in raw material zone B is coaxially aligned with the feed rail 32 in reaction zone C, which is coaxially positioned within the reaction furnace tube 31 in reaction zone C.
[0066] (1) As Figure 19 As shown, the gas supply system A is mainly composed of the following five main parts, namely: gas source, gas circuit valve 55, mass flow controller 54, gas mixer 56 and gas pipeline. The gas source is two or more gases including reaction gas and protective gas. The gas pipeline includes reaction gas pipeline 34 and protective gas pipeline. The gas source of reaction gas is connected to the reaction gas pipeline interface of finished product area D through the gas circuit valve 55, mass flow controller 54, gas mixer 56 and reaction gas pipeline 34. The gas source of protective gas is connected to the protective gas pipeline interface of raw material area B or finished product area D through the gas circuit valve 55, mass flow controller 54 and protective gas pipeline (first protective gas pipeline 22, second protective gas pipeline 38, third protective gas pipeline 39). The reaction gas is delivered to the equipment through the reaction gas pipeline 34, and the protective gas is delivered to the equipment through the protective gas pipeline.
[0067] Gas valve 55 protects mass flow controller 54 and the associated piping by preventing damage caused by prolonged pressure from the gas source. Gas valve 55 can be a plug valve, gate valve, globe valve, or ball valve, and can be made of various metals, inorganic non-metallic materials, or organic polymers.
[0068] The function of the mass flow controller 54 is to control and adjust the input amount of each gas source.
[0069] The function of the gas mixer 56 is to mix gases. It can mix two or more gases simultaneously to prevent excessive stratification of the gases in the pipeline. The gas mixer 56 can be static or dynamic, and its internal structure can be SV, K, SX, SH, SL, SY, or SD.
[0070] The function of the gas pipeline is to transport the source gas to each required gas system. The gas pipeline material can be various metals, inorganic non-metals, and the part outside the high-temperature zone of the system can also be organic polymer material.
[0071] (2) If Figure 2-Figure 8 and Figure 15 、 Figure 18 As shown, the raw material area B is mainly composed of the following main parts, namely: raw material end sealing flange 14, raw material bin 15 (raw material bin outer door 30, raw material bin inner door 28, drive device and sealing gasket), local pushing device (linear slide module 1, linear slide module stable base 2, push end sealing flange 3, linear slide module connecting sleeve 4, magnetic transmission module limit 5, magnetic driven module limit 6, transmission module magnet 7, driven module magnet 8, driven module linear bearing 9, transmission module linear bearing 10, transmission rod 11, transmission connector 12, push plate 13, sleeve 66, connecting plate 67, slider 68), pushing rail 16, water-cooled sealing flange 64, raw material end fixed bracket 17, loading fixture (loading fixture limit bolt 45, loading fixture upper limit sleeve 46, loading fixture lower limit sleeve 47), and material transfer plate 53.
[0072] The raw material bin 15 is installed on the bracket 17, and a horizontal raw material bin outer door 30 is provided at the flange opening at the upper end thereof, and a horizontal raw material bin inner door 28 is provided in the inner cavity of the raw material bin 15 below the raw material bin outer door 30. The chamber formed between the raw material bin outer door 30 and the raw material bin inner door 28 is a raw material bin buffer bin 61. A pushing rail 16 is provided at the bottom of the inner cavity of the raw material bin 15, and the outer wall of the pushing rail 16 is semi-cylindrical and follows the inner wall of the raw material bin 15. The inner wall of the pushing rail 16 is symmetrically provided with a guide rail 65, and the upper part of the guide rail 65 of the pushing rail 16 corresponds to the pushing plate 13 of the local pushing device. A raw material end sealing flange 14 is installed on the side (tail end) of the raw material bin 15 close to the local pushing device, and a water-cooled sealing flange 64 is provided on the other side of the raw material bin 15 at the connection between the raw material bin 15 and the feed end of the reactor tube 31 in the reaction zone C.
[0073] A local pushing device is connected to the tail end of the raw material bin 15. The local pushing device is mainly composed of the following five main parts: a driving module (linear slide module 1, a linear slide module stable base 2, a linear slide module connecting sleeve 4, and a sleeve 66), a transmission module (a magnetic transmission module limit 5, a transmission module NdFeB magnet 7, and a transmission module linear bearing 10), a driven module (a magnetic driven module limit 6, a driven module NdFeB magnet 8, and a driven module linear bearing 9), a pushing module (a transmission rod 11, a transmission connector 12, and a pushing plate 13), and a seal (a pushing end sealing flange 3). The specific structure is as follows:
[0074] The pushing end sealing flange 3 corresponds to the raw material end sealing flange 14 and is sealed and fixed to the tail end of the raw material bin 15 by screws. A sleeve 66 is coaxially integrated with one side of the pushing end sealing flange 3. One end of the transmission rod 11 passes through the raw material end sealing flange 14 and is sealed in the sleeve 66 on one side of the pushing end sealing flange 3. The other end of the transmission rod 11 is connected to the horizontal pushing plate 13 through the transmission connector 12. The pushing plate 13 is in sliding fit with the pushing support rail 16 in the inner cavity of the raw material bin 15.
[0075] The linear slide module connecting sleeve 4 is installed on the sleeve 66. The linear slide module connecting sleeve 4 is connected to the slider 68 on the linear slide module 1 through the connecting plate 67. The linear slide module connecting sleeve 4 slides back and forth on the linear slide module 1 through the slider 68, further driving the transmission rod 11, the transmission connector 12, and the push plate 13 to move.
[0076] The transmission module magnet 7 and the transmission module linear bearing 10 are coaxially arranged between the inner side of the linear slide module connecting sleeve 4 and the sleeve 66, and the magnetic transmission module limit 5 is set at both ends of the transmission module magnet 7 and the transmission module linear bearing 10; the driven module magnet 8 and the driven module linear bearing 9 are coaxially fixed between the outer side of one end of the transmission rod 11 extending into the sleeve 66 and the sleeve 66, and the magnetic driven module limit 6 is set at both ends of the driven module magnet 8 and the driven module linear bearing 9.
[0077] The loading fixture includes a loading fixture limiting bolt 45, a loading fixture upper limit sleeve 46, and a loading fixture lower limit sleeve 47. The loading fixture upper limit sleeve 46 and the loading fixture lower limit sleeve 47 are rectangular frame structures arranged relatively up and down. The material to be reacted 48 is located between the loading fixture upper limit sleeve 46 and the loading fixture lower limit sleeve 47. The loading fixture upper limit sleeve 46 and the loading fixture lower limit sleeve 47 are connected and fixed by the loading fixture limiting bolt 45.
[0078] The material transfer plate 53 is provided with densely packed air holes evenly distributed thereon, and the material transfer plate 53 is disposed on one side of the material to be reacted 48 .
[0079] During use, the material to be reacted 48 is placed directly on the pushing rail 16, or the material to be reacted 48 is clamped by a material loading clamp and placed on the pushing rail 16, or the material transfer plate 53 is placed on the pushing rail 16, and the material to be reacted 48, the material loading clamp or the material transfer plate 53 are pushed to the material transfer guide rail 32 of the reaction zone C by the pushing plate 13.
[0080] The upper flange of the raw material bin 15 and the outer door 30 of the raw material bin are sealed by an O-ring gasket 23, and fastening screw holes 27 are symmetrically opened at the end face of the upper flange of the raw material bin 15. The fasteners pass through the outer door 30 of the raw material bin and the upper flange of the raw material bin 15 and are installed in the fastening screw holes 27, so that the outer door 30 of the raw material bin is sealed and connected to the upper flange of the raw material bin 15.
[0081] The inner door 28 of the raw material bin is installed in the inner cavity of the raw material bin 15 below the outer door 30 of the raw material bin in the form of a plug-in plate. The lower ends of the inner door 28 of the raw material bin are sealed with the side walls of the inner cavity of the raw material bin 15 by square sealing gaskets 24. The upper ends of the inner door 28 of the raw material bin are symmetrically provided with longitudinal pneumatic retractors 25. The pneumatic retractors 25 are connected to the pneumatic retractor air source pipeline 26, and the lifting and lowering of the pneumatic retractor 25 is controlled by the pneumatic retractor air source pipeline 26; the outer end of the inner door 28 of the raw material bin is provided with a screw, and the inner door 28 of the raw material bin is connected to the spiral O-type sealing nut 29 through the screw, and the opening or closing of the inner door 28 of the raw material bin is controlled by the spiral O-type sealing nut 29.
[0082] The function of the raw material bin 15 is to store the materials to be reacted, wherein the outer door 30 of the raw material bin seals the entire raw material bin 15. When the materials to be reacted need to be replenished, the inner door 28 of the raw material bin, the drive device and the sealing gasket work together to isolate and seal the raw material bin buffer bin 61, thereby ensuring that the atmosphere environment of the reaction zone C is not affected by the operation of adding the materials to be reacted.
[0083] The raw material bin 15 contains a raw material buffer bin 61. The outer door 30 (feed bin door) and the inner door 28 (buffer bin door) are compressed by fasteners or pressure using metal gaskets, narrow face seals, self-tightening seals, flat gaskets, Kazari seals, bi-conical seals, Wood's seals, C-shaped seals, or hollow metal O-rings. The inner door 28 (buffer bin door) is pressurized and sealed, and its planar movement is opened and closed by a drive device such as a pull electromagnet, a push electromagnet, or a pneumatic retractor. The gasket can be made of natural rubber, chloroprene rubber, nitrile butadiene rubber, fluororubber, chlorosulfonated polyethylene synthetic rubber, silicone rubber, ethylene propylene rubber, graphite, ceramic fiber, polytetrafluoroethylene, or EPDM sponge. The gasket can have a rectangular cross-section, be metal-wound, flat, corrugated, annular, toothed, triangular, bi-conical, C-shaped, or hollow O-shaped.
[0084] The function of the local pushing device is to cooperate with the pushing support rail 16 and the material transfer guide rail 32 to controllably push the reaction material 48 so that it participates in the reaction and falls into the finished product bin 37 according to the set path.
[0085] The function of the drive module is to provide linear motion power, wherein: the motor in the linear slide module 1 can be a DC motor, a stepper motor, a servo motor or a combination of a motor and a spindle box transmission, and the function of the linear slide module connecting sleeve 4 and sleeve 66 is to provide a reliable mechanical connection for the drive module and the transmission module.
[0086] The function of the transmission module is to transmit power from the outside to the inside, among which: the function of the magnetic transmission module limiter 5 is to limit the position of the transmission module magnet 7 to prevent it from being dislocated during the transmission process; the function of the transmission module magnet 7 is to space the pushing end sealing flange 3 and induction drive the driven module magnet 8; the function of the transmission module linear bearing 10 is to space the transmission module magnet 7 and provide a load-bearing bearing for the relative sliding of the linear slide module connecting sleeve 4 and the pushing end sealing flange 3.
[0087] The function of the driven module is to receive power transmitted from the outside and transmit the power to the pushing module, wherein: the function of the magnetic driven module limiter 6 is to limit the position of the driven module magnet 8 to prevent it from being dislocated during the transmission process; the function of the driven module magnet 8 is to inductively receive the drive of the transmission magnet 7 through the sealing flange 3; the function of the driven module linear bearing 9 is to separate the driven module magnet 8 and provide a load-bearing bearing for the relative sliding of the linear slide module connecting sleeve 4 and the pushing end sealing flange 3.
[0088] The pusher module receives the action of the driven module and moves synchronously with it. The pusher end sealing flange 3 serves to provide a central axis and limit for the driven and pusher modules, and to provide a highly reliable static seal for the driven and pusher modules.
[0089] The materials of the driven module linear bearing 9 and the transmission module linear bearing 10 include but are not limited to stainless steel, zirconium oxide, aluminum oxide, boron nitride, etc.; the materials of the transmission module magnet 7 and the driven module magnet 8 include but are not limited to neodymium iron boron, etc.
[0090] The push rail 16 provides a fixed motion path for the push plate 13, preventing deformation of the transmission rod 11 that could affect its usability during prolonged use. By setting appropriate gaps between the push rail 16, the push plate 13, and the lower edge of the material bin 15, the push process is ensured to be unidirectional and to ensure that only one sample is pushed at a time. The push rail 16 can be made of a variety of materials, including aluminum alloy, magnesium alloy, stainless steel, and quartz.
[0091] The function of the loading fixture (loading fixture limit bolt 45, loading fixture upper limit sleeve 46, loading fixture lower limit sleeve 47) is to clamp the thinner reaction material 48 and participate in the pushing and reaction process together with it. This avoids the sample being subjected to large extrusion stress due to directly pushing the reaction material 48 itself, and avoids the situation where the reaction material 48 is too thin and tilts during the mutual transmission, causing the transmission process to jam or fail. This avoids the problem that when the original amount or remaining amount of reaction material 48 is small, the equipment cannot ensure that each section of raw material can fully pass through the reaction zone and reach the finished product area for collection by simply using the reaction material 48 to transmit to each other. The material of the loading fixture can be aluminum alloy, stainless steel, nickel, copper, graphite or boron nitride, etc., preferably stainless steel or graphite.
[0092] The function of the transfer plate 53 is to provide a push-through for the reacted material. This prevents the problem of the equipment simply using the reacted material 48 to move within the reaction zone, failing to ensure that each section of the material passes through the reaction zone and reaches the finished product area for collection, when the original or remaining amount of reacted material 48 is low. The length, width, and height of the transfer plate 53 are consistent with those of the reacted material / carrying fixture. The material of the transfer plate 53 can be aluminum alloy, stainless steel, nickel, copper, graphite, or boron nitride, with stainless steel or graphite being preferred.
[0093] The function of the water-cooled sealing flange 64 is to cool the sealing ring to prevent the sealing ring from aging and reducing the airtightness.
[0094] The function of the raw material end fixing bracket 17 is to support and fix the raw material bin 15 to ensure the stability of the raw material area of the equipment.
[0095] (3) If Figures 9-12 As shown, the reaction zone C is mainly composed of a tubular heating furnace 57, a reaction furnace tube 31, a feed guide rail 32 and a gas uniform phase distributor 33. The specific structure is as follows: the reaction furnace tube 31 is horizontally arranged in the tubular heating furnace 57, and the feed guide rail 32 is set in the lower half of the inner cavity of the reaction furnace tube 31. The outer wall of the feed guide rail 32 is semi-cylindrical and follows the inner wall of the reaction furnace tube 31. The gas uniform phase distributor 33 is installed at the upper mouth of the feed guide rail 32. The gas uniform phase distributor 33 is an open groove structure, and an air outlet plate 69 is embedded in its upper mouth. The surface of the air outlet plate 69 is densely arranged with gas uniform phase distributor air outlet holes 35. The number of gas uniform phase distributor air outlet holes 35 gradually increases along the air inlet direction, and the aperture of the gas uniform phase distributor air outlet holes 35 gradually increases from the central axis to both sides. The gas uniform phase distributor 33 is connected to the reaction gas pipeline 34 through the gas uniform phase distributor air inlet interface 36 opened on its side.
[0096] The inner cavity of the gas uniform phase distributor 33 is a gas uniform phase distributor uniform gas cavity 63. The gas uniform phase distributor uniform gas cavity 63 is provided with an air inlet channel 70 connected to the gas uniform phase distributor air inlet interface 36. Air dividing cavities 72 are symmetrically arranged on both sides of the air inlet channel 70. The air dividing cavities 72 are open groove structures. A vent 71 is provided on the side of the air dividing cavities 72 corresponding to the air inlet channel 70. The air inlet channel 70 is connected to the air dividing cavities 72 through the vent 71. The vents 71 are arranged according to the rule of gradually becoming larger along the air inlet direction.
[0097] The function of the heating furnace 57 is to provide a stable growth temperature zone for material growth, and the heating temperature range is 100°C to 2500°C, preferably 400°C to 1500°C.
[0098] Reactor tube 31 provides a sealed growth chamber for material growth. Its ends connect to raw material area B and finished product area D, respectively. Flange seals provide a seal to prevent impurities and leakage. Reaction tube 31 can be made of a metal such as quartz, corundum, boron nitride, silicon carbide, high-strength graphite, or stainless steel, with quartz or corundum being preferred.
[0099] A gas uniform distributor cavity 63 is provided inside the gas uniform distributor 33, and the gas uniform distributor cavity 63 is not a simple single-chamber structure. A plurality of mutually interconnected gas partition cavities are provided in the gas uniform distributor cavity 63, and the air vents of the partition cavities are arranged in a rule that gradually increases in size along the air inlet direction. The gas uniform distributor 33 is provided with a plurality of air outlet holes, and the air outlet holes are arranged in a rule that the number of air outlet holes gradually becomes denser along the air inlet direction and the aperture of the air outlet holes gradually becomes larger from the central axis to both sides. The function of the gas uniform distributor 33 is to fully ensure that the reaction gas forms a uniform atmosphere environment in the constant temperature section in the center of the reaction zone after passing through the gas uniform distributor 33, and each position of the prepared material is uniform. The material of the gas uniform distributor 33 can be a metal such as quartz, corundum, boron nitride, silicon carbide, high-strength graphite or stainless steel, preferably graphite or stainless steel.
[0100] The function of the feed rail 32 is to cooperate with the push rail 16 and the local push device to controllably push the reacted materials so that they participate in the reaction and fall into the finished product bin 37 along the set path. The feed rail 32 is a full-length open structure to prevent airflow obstruction and disturbance. In addition, its edges are serrated to achieve the purpose of reducing its contact area with the substrate and air permeability. The material of the feed rail 32 can be quartz, corundum, boron nitride, silicon carbide, high-strength graphite or stainless steel, etc., preferably quartz or corundum.
[0101] (4) If Figure 13-14 As shown, the finished product area D is mainly composed of the following main parts, namely the finished product bin 37 (finished product bin outer door 43, finished product bin inner door 44, drive device and sealing gasket) and the finished product end fixing bracket 17. The specific structure is as follows:
[0102] The finished product bin 37 is mounted on the bracket 17. A horizontal finished product bin outer door 43 is provided at the opening of the flange 42 at the lower end of the finished product bin. A horizontal finished product bin inner door 44 is provided above the finished product bin outer door 43 and within the inner cavity of the finished product bin 37. The chamber formed between the finished product bin outer door 43 and the finished product bin inner door 44 serves as the finished product bin buffer bin 62. A water-cooled sealing flange 64 is provided at the connection between the finished product bin 37 and the discharge end of the reaction furnace tube 31 in the reaction zone C. In addition, the gas supply system A is connected to the reaction gas pipeline interface at the feed end of the finished product bin 37 through the reaction gas pipeline 34, connected to the second shielding gas pipeline 38 at the rear end of the finished product bin 37, and connected to the third shielding gas pipeline 39 on the side of the finished product bin buffer bin 62.
[0103] The lower end flange 42 of the finished product warehouse and the outer door 43 of the finished product warehouse are sealed by an O-ring sealing gasket 23, and fastening screw holes 27 are symmetrically opened at the end face of the lower end flange 42 of the finished product warehouse. The fasteners pass through the outer door 43 of the finished product warehouse and the lower end flange 42 of the finished product warehouse and are installed in the fastening screw holes 27, so that the outer door 43 of the finished product warehouse and the lower end flange 42 of the finished product warehouse are sealed and connected.
[0104] The finished product warehouse inner door 44 is installed in the inner cavity of the finished product warehouse 37 above the finished product warehouse outer door 43 in the form of a plug-in plate. The upper two ends of the finished product warehouse inner door 44 are sealed with the inner cavity side walls of the finished product warehouse 37 by square sealing gaskets 24. The lower two ends of the finished product warehouse inner door 44 are symmetrically provided with longitudinal pneumatic retractors 25. The pneumatic retractor 25 is connected to the pneumatic retractor air source pipeline 26, and the lifting and lowering of the pneumatic retractor 25 is controlled by the pneumatic retractor air source pipeline 26; the outer end of the finished product warehouse inner door 44 is provided with a screw, and the finished product warehouse inner door 44 is connected to the spiral O-type sealing nut 29 through the screw, and the opening or closing of the finished product warehouse inner door 44 is controlled by the spiral O-type sealing nut 29.
[0105] The function of the finished product bin 37 is to store samples that have completed the reaction. The outer door 43 of the finished product bin seals the entire finished product bin 37. When it is necessary to take out the samples that have completed growth, the inner door 44 of the finished product bin, the drive device and the sealing gasket work together to isolate and seal the finished product buffer bin 62, thereby ensuring that the atmosphere of the reaction system is not affected by the operation of taking out the samples that have completed growth.
[0106] Finished product bin 37 contains a finished product buffer bin 62. The finished product bin outer door 43 (receiving bin door) and the finished product bin inner door 44 (buffer bin door) are sealed using fasteners or pressurization, using metal gaskets, narrow face seals, self-tightening seals, flat seals, Kazari seals, biconical seals, Wood seals, C-shaped seals, or hollow metal O-rings. The finished product bin inner door 44 (buffer bin door) is pressurized and sealed, and its planar movement is opened and closed, by a drive device such as a pull electromagnet, a push electromagnet, or a pneumatic retractor. The sealing gasket can be made of natural rubber, chloroprene rubber, nitrile butadiene rubber, fluororubber, chlorosulfonated polyethylene synthetic rubber, silicone rubber, ethylene propylene rubber, graphite, ceramic fiber, polytetrafluoroethylene, or EPDM sponge. The gasket configuration can be rectangular, metal wound, flat, corrugated, annular, toothed, triangular, biconical, C-shaped, or hollow O-shaped.
[0107] The function of the water-cooled sealing flange 64 is to cool the sealing ring to prevent the sealing ring from aging and reducing the sealing degree.
[0108] The function of the protective gas pipeline 38 is to fill the entire equipment cavity with protective atmosphere or to generate a gas barrier through the continuous supply of protective gas during the reaction process, so as to cause the reaction atmosphere to be concentrated in the center of the reaction zone.
[0109] The function of the finished product end fixing bracket 17 is to support and fix the finished product bin 37 to ensure the stability of the finished product bin 37 of the equipment.
[0110] (5) If Figure 16-17 As shown, the exhaust gas and vacuum system E is composed of an exhaust gas system (exhaust gas treatment device, a second check valve 52 and an exhaust gas pipeline, etc.) and a vacuum system (a vacuum pump 49, a first check valve 50, a vacuum pipeline, etc.).
[0111] After connecting to the second check valve 52, the exhaust gas treatment device is tightly connected to the equipment's exhaust gas pipelines (first exhaust gas pipeline 18, second exhaust gas pipeline 20, third exhaust gas pipeline 40, and fourth exhaust gas pipeline 51) via piping. When open, it maintains atmospheric pressure within the entire equipment cavity, or within the raw material bin / raw material buffer bin, or the finished product bin / finished product buffer bin. The exhaust gas treatment device can be one or a combination of two or more of the following: an absorption liquid container 58 (which can contain a solution to neutralize or absorb harmful exhaust gases), a desiccant container 59, and an activated carbon container 60. The absorption liquid container 58 can contain an absorption liquid to neutralize or absorb harmful exhaust gases, the desiccant container 59 can contain a desiccant, and the activated carbon container 60 can contain activated carbon.
[0112] After connecting to the first check valve 50, vacuum pump 49 is tightly connected to the equipment's vacuum lines (first vacuum line 19, second vacuum line 21, and third vacuum line 41) via piping. When activated, it creates a negative pressure growth environment in the equipment or removes air or reactant gases from the entire sealed chamber or raw material buffer bin to ensure a pure and safe reaction process. The vacuum pump can be a dry screw vacuum pump, a water ring pump, a reciprocating pump, a sliding valve pump, a rotary vane pump, a Roots pump, or a diffusion pump.
[0113] The drawings and embodiments described in this specification describe specific implementation methods of the present invention in detail. The following embodiments are used to illustrate the present invention but are not intended to limit the scope of the present invention.
[0114] Example 1
[0115] In this embodiment, a chemical vapor deposition reaction device suitable for uniform and continuous preparation of porous macroscopic materials is provided, including: a linear slide module 1, a linear slide module stable base 2, a push end sealing flange 3, a linear slide module connecting sleeve 4, a magnetic transmission module limit 5, a magnetic driven module limit 6, a transmission module magnet 7, a driven module magnet 8, a driven module linear bearing 9, a transmission module linear bearing 10, a transmission rod 11, a transmission connector 12, a push plate 13, a raw material end sealing method Lantern 14, raw material bin 15, push rail 16, bracket 17, first exhaust gas pipeline 18, first vacuum pipeline 19, second exhaust gas pipeline 20, second vacuum pipeline 21, first protective gas pipeline 22, O-type sealing gasket 23, square sealing gasket 24, pneumatic expansion joint 25, pneumatic expansion joint gas source pipeline 26, fastening screw hole 27, raw material bin inner door 28, sealing nut 29, raw material bin outer door 30, reaction furnace tube 31, material transfer guide rail 32, gas phase distributor 33, reaction gas pipeline 34 , gas uniform phase distributor outlet 35, gas uniform phase distributor air inlet interface 36, finished product bin 37, second protective gas pipeline 38, third protective gas pipeline 39, third tail gas pipeline 40, third vacuum pipeline 41, finished product bin lower end flange 42, finished product bin outer door 43, finished product bin inner door 44, loading fixture limit bolt 45, loading fixture upper limit sleeve 46, loading fixture lower limit sleeve 47, material to be reacted 48, vacuum pump 49, first check valve 50, fourth tail gas pipeline 51, second check valve Valve 52, material transfer plate 53, mass flow controller 54, gas circuit valve 55, gas mixer 56, tubular heating furnace 57, absorption liquid container 58, desiccant container 59, activated carbon container 60, raw material buffer bin 61, finished product buffer bin 62, gas uniform phase distributor uniform gas cavity 63, water-cooled sealing flange 64, guide rail 65, sleeve 66, connecting plate 67, slider 68, gas outlet plate 69, air inlet channel 70, vent 71, gas separation cavity 72, the specific structure, connection and position relationship are as follows: Figure 1-19 shown.
[0116] The usage process of this embodiment is as follows: Start the linear slide module 1 to move the slider in the module to the starting end (the motor direction is the starting direction), ensuring that the front end of the push plate 13 is behind the rear end of the raw material bin 15 (close to the motor direction). Control the pneumatic retractor 25 in the raw material bin 15 to be in a retracted state, loosen the raw material bin sealing nut 29, open the raw material bin inner door 28 horizontally, remove the screws in the finished product bin fastening screw holes 27, open the raw material bin outer door 30, and tighten the raw material bin sealing nut 29. Place multiple pieces of reaction materials 48 (raw materials) into the raw material bin 15, with the bottom layer of reaction materials supported on the push rail 16. Close the raw material bin outer door 30, and insert the screws into the fastening screw holes 27 to tighten the raw material bin outer door 30. Close all gas valves, start the vacuum pump 49, open the valves of the first vacuum line 19, the second vacuum line 21, and the third vacuum line 41, and evacuate the equipment. After the system reaches the required vacuum level, close the valves of the first vacuum line 19, the second vacuum line 21, and the third vacuum line 41 and the vacuum pump 49. Open the valves of the first shielding gas line 22, the second shielding gas line 38, and the third shielding gas line 39 to introduce shielding gas. After each part reaches positive pressure, open the valves of the first tail gas line 18, the second tail gas line 20, and the third tail gas line 40. After each part returns to normal pressure, close the valves of the first shielding gas line 22, the second shielding gas line 38, the second tail gas line 20, and the third tail gas line 40. Open the third shielding gas line 39 and the first tail gas line 18, and use the mass flow controller 54 to control the flow of shielding gas. The tubular heating furnace 57 is turned on to heat the reaction zone. Once the furnace reaches the set temperature, the linear slide module is programmed. The linear slide module, connected to the outer sleeve 4, drives the transmission module and the driven module, causing the pusher plate 13 to move forward and backward in a straight line. As the pusher plate 13 moves forward at the set speed, its front end pushes the bottom layer of the reacted material 48 forward at the same speed. When the front end of the pusher plate 13 just passes the front end of the raw material bin 15 (toward the heating furnace), the program controls the pusher plate 13 to stop moving forward and then withdraw backward at a faster speed to the starting point. At this time, the next piece of reacted material will fall onto the push rail 16, completing the push operation. The above push process is repeated, and the reaction gas and shielding gas are set to the desired flow rate through the corresponding mass flow controller 54. When the first piece of reacted material reaches the edge of the gas phase distributor 33, while the third shielding gas line 39 continues to be opened, the valve of the reaction gas line 34 connected to the gas phase distributor 33 is opened, and the reacted material begins to grow continuously and controllably. When the finished product is pushed to the end of the reaction end, it will fall into the finished product bin 37.When the number of finished products reaches the upper limit, samples are removed. The pneumatic expander 25 in the finished product bin is retracted. The finished product bin sealing nut 29 is loosened, the inner door 44 is opened horizontally, and the finished product bin sealing nut 29 is tightened. The finished products fall onto the outer door 43. The finished product bin sealing nut 29 is loosened, the inner door 44 is closed horizontally, and the finished product bin sealing nut 29 is tightened. The pneumatic expander 25 in the finished product bin is extended. The vacuum pump 49 is started, the valve of the third vacuum line 41 is opened, and the finished product buffer bin 62 is evacuated. Once the required vacuum level is reached, the valve of the third vacuum line 41 and the vacuum pump 49 are closed. The valve of the third protective gas line 39 is opened. After the finished product buffer bin 62 reaches positive pressure, the valve of the third exhaust gas line 40 is opened. After the finished product buffer bin 62 reaches normal pressure, the valves of the third protective gas line 39 and the third exhaust gas line 40 are closed. Remove the screws from the fastening screw holes 27 of the finished product bin, open the outer door 43 of the finished product bin, take out the finished product, close the outer door 43 of the finished product bin, and insert the screws into the fastening screw holes 27 of the finished product bin to tighten and seal. Open the valve of the third vacuum line 41, evacuate the finished product bin 37, and close the valve of the third vacuum line 41 and the vacuum pump 49 after reaching the vacuum degree. Open the valve of the third protective gas line 39, and after the finished product bin buffer bin 62 reaches positive pressure, open the valve of the third tail gas line 40. After the finished product bin buffer bin 62 reaches normal pressure, close the valves of the third protective gas line 39 and the third tail gas line 40. At this point, a sampling operation is completed without affecting the normal reaction of the reaction zone. When new materials to be reacted need to be added: loosen the sealing nut 29 of the raw material bin, close the inner door 28 of the raw material bin horizontally, tighten the sealing nut 29 of the raw material bin, and control the pneumatic retractor 25 in the raw material bin 15 to be in the extended state. Start the vacuum pump 49, open the valve of the second vacuum line 21, and evacuate the raw material buffer chamber 61. Once the desired vacuum level is reached, close the valve of the second vacuum line 21 and the vacuum pump 49. Open the valve of the first shielding gas line 22. Once the raw material buffer chamber 61 reaches positive pressure, open the valve of the second tail gas line 20. Once the raw material buffer chamber 61 reaches normal pressure, close the valves of the first shielding gas line 22 and the second tail gas line 20. Remove the screws from the fastening screw holes 27 of the raw material bin 15, open the raw material bin outer door 30, and place the reacted material 48 into the raw material bin buffer chamber 61 of the raw material bin 15. The material is temporarily loaded onto the raw material bin inner door 28. Close the raw material bin outer door 30, and insert the screws into the finished product bin fastening screw holes 27 to secure and seal the material. Open the valve of the second vacuum line 21, evacuate the raw material buffer chamber 61, and once the desired vacuum level is reached, close the valve of the second vacuum line 21 and the vacuum pump 49. Open the valve of the first protective gas pipeline 22, and after the raw material warehouse buffer warehouse 61 reaches positive pressure, open the valve of the second tail gas pipeline 20. After the raw material warehouse buffer warehouse 61 reaches normal pressure, close the valves of the first protective gas pipeline 22 and the second tail gas pipeline 20.Control the pneumatic expansion joint 25 in the raw material bin 15 to its retracted position, loosen the raw material bin sealing nut 29, open the internal door 28 horizontally, and tighten the raw material bin sealing nut 29. The reactant material will then fall onto the reactant material already in the bin. This completes the feeding operation without disrupting the normal reaction in the reaction zone. This operation allows for uninterrupted, continuous, and uniform growth of the desired material.
[0117] Example 2
[0118] The equipment structure and most of the operating steps of this embodiment are the same as those of Example 1. The difference is that in Example 1, the material to be reacted 48 directly participates in the preparation process during the reaction process. In this embodiment, the material to be reacted 48 is a segmented thin layer substrate, which is not suitable for direct pushing. During the preparation stage, it is necessary to place the material to be reacted 48 on the lower limit sleeve 47 of the loading fixture. The upper limit sleeve 46 of the loading fixture is aligned with the corresponding position of the lower limit sleeve 47 of the loading fixture and covered on the material to be reacted 48. The loading fixture limit pin 45 is inserted into the corresponding hole to complete the limit clamping of the material to be reacted 48. The loading fixture (loading fixture limit pin 45, loading fixture upper limit sleeve 46, loading fixture lower limit sleeve 47) and the material to be reacted 48 are then used as a whole to participate in the preparation process.
[0119] Example 3
[0120] The equipment structure and most operational steps of this embodiment are identical to those of Example 1. The difference is that Example 1 is applicable when there is a sufficient amount of reacted material 48 and the equipment still has a long scheduled operating time. This embodiment, however, is primarily designed to address situations where the initial or remaining amount of reacted material 48 is low, or when the equipment requires maintenance or overhaul. In this embodiment, a certain amount of reacted material 48 or the carrier fixture (carrier fixture stop bolt 45, carrier fixture upper limit sleeve 46, carrier fixture lower limit sleeve 47) plus reacted material 48 can be replaced with the transfer plate 53 as needed. This ensures that, in these situations, each section of reacted material 48 can still fully pass through the reaction zone and reach the finished product area for collection.
[0121] The embodiments of the present invention do not limit the present invention. The various components of the device may be modified and improved in a number of ways. Such modifications and improvements without departing from the technical principles of the present invention should also be considered within the scope of protection of the present invention.
Claims
1. A chemical vapor deposition reaction device suitable for uniform and continuous large-area preparation of segmented membrane materials, characterized in that: The equipment consists of a gas supply system, a raw material area, a reaction area, a finished product area, and an exhaust and vacuum system. The specific structure is as follows: The raw material bin in the raw material area is connected to the feed end of the reactor tube in the reaction area, and the finished product bin in the finished product area is connected to the discharge end of the reactor tube in the reaction area; the gas supply system is connected to the protective gas pipeline interface in the raw material area through the first protective gas pipeline, the gas supply system is connected to the protective gas pipeline interface in the finished product area through the second protective gas pipeline and the third protective gas pipeline, and the gas supply system is connected to the reaction gas pipeline interface in the finished product area through the reaction gas pipeline; the vacuum pump of the tail gas and vacuum system is connected to the vacuum pipeline interface in the raw material area through the first vacuum pipeline and the second vacuum pipeline respectively, and the vacuum pump of the tail gas and vacuum system is connected to the vacuum pipeline interface in the finished product area through the third vacuum pipeline; the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface in the raw material area through the first tail gas pipeline and the second tail gas pipeline after passing through the second check valve, the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface in the finished product area through the third tail gas pipeline after passing through the second check valve, and the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface of the vacuum system through the fourth tail gas pipeline after passing through the second check valve; A raw material buffer bin is provided above the raw material bin in the raw material area, and a finished product buffer bin is provided below the finished product bin in the finished product area; the push rail in the raw material area is coaxially aligned with the feed guide rail in the reaction area, and the feed guide rail is coaxially placed in the reaction furnace tube in the reaction area; The raw material bin in the raw material area is installed on the bracket, and a horizontal raw material bin outer door is provided at the flange opening at the upper end thereof, and a horizontal raw material bin inner door is provided below the raw material bin outer door in the inner cavity of the raw material bin, and the chamber formed between the raw material bin outer door and the raw material bin inner door is the raw material bin buffer bin, and a pushing rail is provided at the bottom of the inner cavity of the raw material bin, and the outer wall of the pushing rail is semi-cylindrical and follows the shape of the inner wall of the raw material bin, and the inner wall of the pushing rail is symmetrically provided with a guide rail, and the upper part of the guide rail of the pushing rail corresponds to the pushing plate of the local pushing device, and a raw material end sealing flange is provided on the side of the raw material bin close to the local pushing device, and a water-cooled sealing flange is provided on the other side of the raw material bin at the connection between the raw material bin and the feed end of the reactor tube in the reaction zone; A local push device is connected to the tail end of the raw material warehouse. The specific structure of the local push device is as follows: The sealing flange at the push end corresponds to the sealing flange at the raw material end and is sealed and fixed to the tail end of the raw material bin by screws. A sleeve is coaxially integrated on one side of the sealing flange at the push end. One end of the transmission rod passes through the sealing flange at the raw material end and is sealed in the sleeve on one side of the sealing flange at the push end. The other end of the transmission rod is connected to the horizontal push plate through a transmission connector. The push plate is in sliding cooperation with the push rail in the inner cavity of the raw material bin. The sleeve is equipped with a linear slide module connecting sleeve, which is connected to the slider on the linear slide module through a connecting plate. The linear slide module connecting sleeve slides back and forth on the linear slide module through the slider, further driving the transmission rod, transmission connector, and push plate to move; The transmission module magnet and the transmission module linear bearing are coaxially arranged between the inner side of the linear slide module connecting sleeve and the sleeve, and magnetic transmission module limiters are set at both ends of the transmission module magnet and the transmission module linear bearing; the driven module magnet and the driven module linear bearing are coaxially fixed between the outer side of one end of the transmission rod extending into the sleeve and the sleeve, and magnetic driven module limiters are set at both ends of the driven module magnet and the driven module linear bearing; The reaction zone includes a tubular heating furnace, a reaction furnace tube, a feed guide rail and a gas uniform phase distributor. The specific structure is as follows: the reaction furnace tube is horizontally arranged in the tubular heating furnace, the feed guide rail is arranged in the lower half of the inner cavity of the reaction furnace tube, the outer wall of the feed guide rail is semi-cylindrical and follows the inner wall of the reaction furnace tube, the gas uniform phase distributor is installed at the upper opening of the feed guide rail, the gas uniform phase distributor is an open groove structure, the upper opening of which is embedded with a gas outlet plate, the surface of the gas outlet plate is densely arranged with gas outlet holes of the gas uniform phase distributor, the number of gas outlet holes of the gas uniform phase distributor gradually increases along the air inlet direction, and the aperture of the gas outlet holes of the gas uniform phase distributor gradually increases from the central axis to both sides. The gas uniform phase distributor is connected to the reaction gas pipeline through the gas uniform phase distributor air inlet interface opened on its side; The inner cavity of the gas uniform phase distributor is a gas uniform phase distributor gas uniform cavity. The gas uniform phase distributor gas uniform cavity is provided with an air inlet channel connected to the air inlet interface of the gas uniform phase distributor. Air dividing cavities are symmetrically arranged on both sides of the air inlet channel. The air dividing cavities are open groove structures. A vent is provided on the side of the air dividing cavities corresponding to the air inlet channel. The air inlet channel is connected to the air dividing cavities through the vent. The vents are arranged according to the rule of gradually becoming larger along the air inlet direction.
2. The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials according to claim 1, characterized in that: The gas supply system includes a gas source, a gas circuit valve, a mass flow controller, a gas mixer and a gas pipeline. The specific structure is as follows: the gas source is two or more gases including reaction gas and protective gas, and the gas pipeline includes a reaction gas pipeline and a protective gas pipeline. The gas source of the reaction gas is connected to the reaction gas pipeline interface of the finished product area through the gas circuit valve, the mass flow controller, the gas mixer, and the reaction gas pipeline. The gas source of the protective gas is connected to the protective gas pipeline interface of the raw material area or the finished product area through the gas circuit valve, the mass flow controller, and the protective gas pipeline. The reaction gas pipeline transports reaction gas to the equipment, and the protective gas pipeline transports protective gas to the equipment; the gas mixer mixes two or more gases at the same time to prevent gas stratification in the pipeline; the gas mixing method of the gas mixer is static mixing or dynamic mixing, and its internal structure is SV type, K type, SX type, SH type, SL type, SY type or SD type.
3. The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials according to claim 1, characterized in that: The outer door and the inner door of the raw material bin are compressed by fasteners or pressurization to form metal gaskets, narrow face seals, self-tightening seals, flat gasket seals, Kazari seals, double cone seals, Wood seals, C-type seals or hollow metal O-ring seals; the inner door of the raw material bin is pressurized and sealed and opened and closed by planar movement by one of the pull-type electromagnets, push-type electromagnets or pneumatic retractors.
4. The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials according to claim 1, characterized in that: The upper flange of the raw material bin and the outer door of the raw material bin are sealed by an O-ring gasket, and fastening screw holes are symmetrically opened on the end face of the upper flange of the raw material bin. Fasteners pass through the outer door of the raw material bin and the upper flange of the raw material bin and are installed in the fastening screw holes, so that the outer door of the raw material bin and the upper flange of the raw material bin are sealed and connected; The raw material warehouse is installed in the form of a plug-in plate in the inner cavity of the raw material warehouse below the outer door of the raw material warehouse. The lower ends of the inner door of the raw material warehouse are sealed with the side walls of the inner cavity of the raw material warehouse by square sealing gaskets. The upper ends of the inner door of the raw material warehouse are symmetrically arranged with longitudinal pneumatic expanders. The pneumatic expanders are connected to the pneumatic expander air source pipeline, and the lifting of the pneumatic expander is controlled by the pneumatic expander air source pipeline; the outer end of the inner door of the raw material warehouse is provided with a screw, and the inner door of the raw material warehouse is connected to the spiral O-type sealing nut through the screw, and the opening or closing of the inner door of the raw material warehouse is controlled by the spiral O-type sealing nut.
5. The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials according to claim 1, characterized in that: The material to be reacted is placed directly on the push rail, or the material to be reacted is placed on the push rail after being clamped by a material loading fixture, or the material transfer plate is placed on the push rail; The loading fixture includes a loading fixture limit bolt, an upper limit sleeve of the loading fixture, and a lower limit sleeve of the loading fixture. The upper limit sleeve of the loading fixture and the lower limit sleeve of the loading fixture are rectangular frame structures arranged relatively up and down. The material to be reacted is located between the upper limit sleeve of the loading fixture and the lower limit sleeve of the loading fixture. The upper limit sleeve of the loading fixture and the lower limit sleeve of the loading fixture are connected and fixed by the loading fixture limit bolt; the material transfer plate is arranged on one side of the material to be reacted, and the material transfer plate is evenly and densely arranged with air holes.
6. The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials according to claim 1, characterized in that: The finished product bin in the finished product area is installed on the bracket, and a horizontal finished product bin outer door is provided at the flange opening at the lower end of the finished product bin. A horizontal finished product bin inner door is provided above the finished product bin outer door in the inner cavity of the finished product bin. The chamber formed between the finished product bin outer door and the finished product bin inner door is the finished product bin buffer bin. A water-cooled sealing flange is provided at the connection between the finished product bin and the discharge end of the reaction furnace tube in the reaction zone; the gas supply system is connected to the reaction gas pipeline interface at the feed end of the finished product bin through the reaction gas pipeline, is connected to the second protective gas pipeline at the tail end of the finished product bin, and is connected to the third protective gas pipeline on the side of the finished product bin buffer bin; The lower flange of the finished product bin and the outer door of the finished product bin are sealed by an O-ring gasket, and fastening screw holes are symmetrically opened on the end face of the lower flange of the finished product bin. Fasteners pass through the outer door of the finished product bin and the lower flange of the finished product bin and are installed in the fastening screw holes, so that the outer door of the finished product bin and the lower flange of the finished product bin are sealed and connected; The inner door of the finished product warehouse is installed in the inner cavity of the finished product warehouse above the outer door of the finished product warehouse in the form of a plug-in plate. The upper two ends of the inner door of the finished product warehouse are sealed with the side walls of the inner cavity of the finished product warehouse by square sealing gaskets. The lower two ends of the inner door of the finished product warehouse are symmetrically provided with longitudinal pneumatic expanders, which are connected to the pneumatic expander air source pipeline, and the lifting and lowering of the pneumatic expander are controlled by the pneumatic expander air source pipeline; the outer end of the inner door of the finished product warehouse is provided with a screw, and the inner door of the finished product warehouse is connected to the spiral O-type sealing nut through the screw, and the opening or closing of the inner door of the finished product warehouse is controlled by the spiral O-type sealing nut.
7. The chemical vapor deposition reaction equipment suitable for uniform and continuous large-area preparation of segmented membrane materials according to claim 1, characterized in that: The tail gas and vacuum system includes a tail gas system and a vacuum system. The tail gas system is provided with a tail gas treatment device, a second check valve and a tail gas pipeline. The vacuum system is provided with a vacuum pump, a first check valve and a vacuum pipeline. The tail gas treatment device is connected to the second check valve and is closely connected to the equipment tail gas pipeline through a pipeline. When it is opened, it maintains the entire equipment cavity or the raw material warehouse / raw material buffer warehouse, finished product warehouse / finished product buffer warehouse at normal pressure. The tail gas treatment device is one or a combination of two or more of an absorption liquid container, a desiccant container, and an activated carbon container. A solution for neutralizing or absorbing harmful tail gas is added to the absorption liquid container, a desiccant is added to the desiccant container, and activated carbon is added to the activated carbon container. The vacuum pump is connected to the first check valve and is tightly connected to the equipment vacuum pipeline through a pipeline. When turned on, it realizes a negative pressure growth environment of the equipment or absorbs the air or reaction gas in the entire sealed cavity or raw material buffer bin. The vacuum pump is a dry screw vacuum pump, a water ring pump, a reciprocating pump, a sliding valve pump, a rotary vane pump, a Roots pump or a diffusion pump.
Citation Information
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