A chemical vapor deposition reaction device suitable for uniform, continuous and efficient preparation of porous macroscopic materials

Abstract

The present invention relates to the field of chemical vapor deposition reaction equipment, specifically a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials. The equipment is composed of an air intake control system, a feeding system, a reaction system, a receiving system, and an exhaust gas and vacuum system. The air intake control system is connected to the feeding system and the receiving system through a protective gas pipeline, and is connected to the receiving system through a reaction gas pipeline; the feeding system is provided with a local conveying crawler, and a feeding buffer bin is provided on the upper part of the feeding bin of the feeding system. The slit in the middle of the inner lining cavity of the reaction system is coaxially aligned with the local conveying crawler of the feeding system, and a receiving buffer bin is provided on the lower part of the receiving bin of the receiving system. The vacuum system and the exhaust gas system of the exhaust gas and vacuum system are respectively connected to the feeding system and the receiving system. The present invention ensures that each position in the continuous preparation process of porous bulk materials can experience the same uniform and efficient growth environment, breaking through the material size, especially the length limitation.

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, continuous and efficient preparation of porous macroscopic materials. Background Art

[0002] Chemical vapor deposition (CVD) is one of the main methods for the large-scale, controllable preparation of new materials such as graphene and boron nitride. 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 accurately 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 a specific substrate (especially a catalytically active metal substrate) and temperature and 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 bulk porous materials, which seriously hinders the further application and development of this technology: (1) 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. (2) 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 cause a great safety hazard and seriously affect the quality of the prepared material due to the infiltration of impurity gases such as oxygen in the air. For airtightness considerations, general chemical vapor deposition devices can only adopt the reaction mode of sample heating and cooling with the furnace, which is very time-consuming and energy-consuming. (3) Although some CVD equipment also has a push-pull rod that runs through the reaction zone to send samples 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 materials, 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. It is difficult to effectively ensure the airtightness of the system under a dynamic sealing environment. At the same time, an overly long push-pull rod takes up a lot of space and 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. (4) 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 adding or removing materials, more than two cycles of evacuating / emptying the reaction gas-filling the protective gas operation are still required, which makes it impossible to achieve continuous loading and collection of samples, and the production efficiency is still low. Although some equipment is equipped with simple feeding and receiving bins, due to the lack of a buffer bin and an automatically controlled sealing plate valve design, it can only achieve batch feeding and collection, which cannot truly achieve an uninterrupted, continuous, and automated reaction process. (5) Although some growth equipment uses a conveying crawler structure that runs through the entire furnace tube cavity and is directly or indirectly driven by an external motor in order to achieve continuous sample transmission (which also faces the airtightness problem described in Article 3), it is not possible to achieve continuous sample transmission. However, on the one hand, since the conveyor belt needs to pass through the high temperature zone (the temperature can be as high as thousands of degrees Celsius) and the reaction atmosphere environment, 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 significant deformation caused by the thermal expansion and contraction of the conveyor belt throughout the entire furnace tube cavity due to the drastic temperature changes during the transmission process (the temperature difference between the normal temperature zone and the high temperature zone can be as high as thousands of degrees Celsius) 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 conveyor belt structure of the circular transmission will greatly occupy the space inside the furnace tube, limit the size of the sample accommodated (especially in the width direction), and cause significant disturbances to the temperature and airflow in the reaction zone, seriously affecting the uniformity and quality of the prepared material. (6) The atmosphere required for general chemical vapor deposition reactions 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 densities and proportions of different gases, under the influence of gravity and gas flow rate, the atmosphere environment at different positions of the CVD process reaction zone (for example, front and back, up and down) is significantly different, making it difficult to ensure the uniformity of the prepared materials; at the same time, the open growth environment of the entire furnace tube also means that most of the reaction gases do not come into contact with the sample to participate in the reaction but are directly discharged through the exhaust gas, which not only causes serious waste, but is also not conducive to the reaction gas fully contacting and penetrating the porous bulk material, and is not conducive to achieving uniform and efficient 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 the uniform, continuous and efficient preparation of porous macroscopic materials, which realizes the precise transmission and continuous preparation of materials under ultra-high airtightness, ensures that the porous bulk phase materials can continuously experience the same uniform and efficient growth environment at each position during the preparation process, and the reaction process is continuous, uniform, 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 device suitable for uniform, continuous and efficient preparation of porous macroscopic materials. The device consists of an air intake control system, a feeding system, a reaction system, a material collection system, and an exhaust and vacuum system. The specific structure is as follows:

[0007] The feed bin of the feeding system is connected to the feeding end of the reaction furnace tube of the reaction system, and the receiving bin of the receiving system is connected to the discharging end of the reaction furnace tube of the reaction system; the air intake control system is connected to the protection gas pipeline interface of the feeding system through the first protection gas pipeline, the air intake control system is connected to the protection gas pipeline interface of the receiving system through the second protection gas pipeline and the third protection gas pipeline, and the air intake control system is connected to the reaction gas pipeline interface of the receiving system through the reaction gas pipeline; the vacuum system of the tail gas and vacuum system is connected to the vacuum pipeline interface of the feeding system through the first vacuum pipeline and the second vacuum pipeline respectively, and the vacuum system of the tail gas and vacuum system is connected to the vacuum pipeline interface of the receiving system through the third vacuum pipeline; the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface of the feeding system through the first tail gas pipeline and the second tail gas pipeline, the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface of the receiving system through the third tail gas pipeline and / or the fourth tail gas pipeline, 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 fifth tail gas pipeline;

[0008] The feeding system is provided with a local conveying crawler installed on the crawler wheel, a feeding buffer bin is provided on the upper part of the feeding bin of the feeding system, the middle material passing slit of the inner lining cavity of the reaction system is coaxially aligned with the local conveying crawler of the feeding system, and a receiving buffer bin is provided on the lower part of the receiving bin of the receiving system.

[0009] The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials, the air intake control system includes a gas source, an air 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 receiving system through the air circuit valve, the mass flow controller, the gas mixer, the reaction gas pipeline, and the protective gas pipeline is connected to the protective gas pipeline interface of the feeding system or the receiving system through the air circuit valve, the mass flow controller, the protective gas pipeline, the reaction gas pipeline transports the reaction gas to the equipment, and the protective gas pipeline transports the protective gas to the equipment.

[0010] The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials is characterized in that a gas mixer simultaneously mixes two or more gases to prevent excessive stratification of the gases in the pipeline; the gas flow rate is adjusted by a mass flow controller through closed-loop control, and then fully mixed through the gas mixer and transported to the reaction chamber of the reaction system; 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.

[0011] The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials is described. The feed bin of the feeding system is installed on a bracket, and a horizontal feed bin first-level bin door is provided at the opening of the upper end thereof. A horizontal feed bin second-level bin door is provided below the first-level bin door in the inner cavity of the feed bin. The chamber formed between the first-level bin door and the second-level bin door is a feed buffer bin. An observation window is provided on one side of the feed bin, and a sealing ring cooling jacket is provided on the other side of the feed bin at the connection between the feed bin and the feed end of the reaction furnace tube of the reaction system; a crawler installed on a track wheel is provided in the inner cavity of the feed bin below the second-level bin door. The power of the track wheel is generated by a driving motor, and the power is transmitted from the outside to the inside for closed transmission through a radial magnetic coupling coupling. The track wheel is powered by gears, screws or direct connections. The track adopts friction transmission or meshing transmission. The driving motor is a DC motor, a stepping motor, a servo motor or a combination of a motor and a spindle box transmission.

[0012] The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials is characterized in that the main gear is transmitted to the track wheel through the steering transmission gear pair fixed in the fixed bearing, one end of the transmission shaft passes through the fixed bearing and is connected with the steering transmission gear pair, the vertical steering transmission gear pair is engaged with the horizontal active gear, the output end of the drive motor is connected with the active gear, the steering transmission gear pair is coaxially connected to the center of the track wheel through the other end of the transmission shaft, and drives the track wheel to rotate, and the clockwise / counterclockwise controllable rotation of the track wheel drives the track to move forward / backward at a set speed; material limit blocks are set on the surface of the track, and the material limit blocks are distributed on half of the track surface.

[0013] The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials, the first-level door and the second-level door of the feed bin rely on fasteners or pressurization to compress metal gaskets for sealing, 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, and the second-level door of the feed bin is pressurized and sealed and opened and closed by planar motion by one of a pull electromagnet, a push electromagnet or a push-pull cylinder.

[0014] The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials is sealed between the upper flange of the feed bin and the first-level bin door of the feed bin by a square flexible sealing gasket, and fastener holes are symmetrically opened on the end face of the upper flange of the feed bin. The fasteners pass through the first-level bin door of the feed bin and the upper flange of the feed bin and are installed in the fastener holes, so that the first-level bin door of the feed bin is sealed and connected to the upper flange of the feed bin;

[0015] The secondary door of the feed bin is installed in the inner cavity of the feed bin below the primary door of the feed bin in the form of a plug-in plate. The lower ends of the secondary door of the feed bin are sealed with the side walls of the inner cavity of the feed bin by O-type flexible sealing gaskets. The upper ends of the secondary door of the feed bin are symmetrically provided with longitudinal push-pull cylinders, which are connected to the push-pull cylinder air circuit, and the lifting and lowering of the push-pull cylinder is controlled by the push-pull cylinder air circuit; a screw is provided at the outer end of the secondary door of the feed bin, which is connected to the spiral O-type fastening nut group through the screw, and the opening or closing of the secondary door of the feed bin is controlled by the spiral O-type fastening nut group.

[0016] The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials, the reaction system includes a heating furnace, a reaction furnace tube and an inner lining cavity, the inner lining cavity is a three-region combination structure, including a reaction chamber gas supply area, a reaction chamber uniform gas reaction area and a reaction chamber track area, the reaction furnace tube is arranged in the heating furnace in a horizontal direction, and the inner cavity of the reaction furnace tube is sequentially provided with a cylindrical reaction chamber gas supply area, a reaction chamber uniform gas reaction area and a reaction chamber track area, the outer end of the reaction chamber gas supply area corresponds to the material receiving system, the outer end of the reaction chamber track area corresponds to the material feeding system, the reaction chamber gas supply area, the reaction chamber uniform gas reaction area and the reaction chamber track area A strip-shaped material passing slit is opened in the middle of the channel area in the horizontal direction as a material limiting track. The cross-sectional dimensions of the three material limiting tracks are the same and interconnected. Horizontal gas pipelines are opened above and below the material limiting tracks of the reaction chamber gas supply area and the reaction chamber uniform gas reaction area. Local uniform phase air holes are opened above and below the material limiting tracks of the reaction chamber uniform gas reaction area. The arrangement of the local uniform phase air holes is non-uniform. The number of local uniform phase air holes gradually becomes denser from the center to the two sides, and the aperture gradually expands. The reaction chamber gas supply area, the reaction chamber uniform gas reaction area and the reaction chamber track area are connected by threaded connections or straight plug connections.

[0017] The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials is described. The receiving bin of the receiving system is installed on a bracket, and a horizontal first-level bin door of the receiving bin is provided at the opening of the lower end thereof. A horizontal second-level bin door of the receiving bin is provided above the first-level bin door in the inner cavity of the receiving bin. The chamber formed between the first-level bin door and the second-level bin door of the receiving bin is a receiving buffer bin. A sealing ring cooling jacket is provided at the connection between the receiving bin and the discharge end of the reaction furnace tube of the reaction system, and a material guide plate is provided at the feed end of the receiving bin; a reaction gas pipeline is symmetrically provided on the flange at one end of the receiving bin, or a fourth tail gas pipeline and a reaction gas pipeline are symmetrically provided on the flange at one end of the receiving bin; a protective gas pipeline is provided on the flange at the other end of the receiving bin, and protective gas is controllably and continuously supplied through the protective gas pipeline during the reaction process to form a gas barrier at the receiving end of the equipment;

[0018] The lower flange of the receiving bin and the first-level bin door of the receiving bin are sealed by a square flexible sealing gasket, and the end face of the lower flange of the receiving bin is symmetrically opened with fastener holes. The fasteners pass through the first-level bin door of the receiving bin and the lower flange of the receiving bin and are installed in the fastener holes, so that the first-level bin door of the receiving bin is sealed and connected with the lower flange of the receiving bin;

[0019] The secondary door of the receiving bin is installed in the inner cavity of the receiving bin above the primary door of the receiving bin in the form of a plug-in plate. The upper two ends of the secondary door of the receiving bin are sealed with the side walls of the inner cavity of the receiving bin by O-type flexible sealing gaskets. The lower two ends of the secondary door of the receiving bin are symmetrically arranged with longitudinal push-pull cylinders, which are connected to the push-pull cylinder air circuit, and the lifting and lowering of the push-pull cylinder is controlled by the push-pull cylinder air circuit; a screw is provided at the outer end of the secondary door of the receiving bin, which is connected to the spiral O-type fastening nut group through the screw, and the opening or closing of the secondary door of the receiving bin is controlled by the spiral O-type fastening nut group.

[0020] The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic 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. The vacuum system is provided with a vacuum pump, a first check valve and a vacuum pipeline. The specific structure is as follows:

[0021] 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, the entire cavity of the equipment or the feed bin / feed buffer bin and the receiving bin / receiving buffer bin are maintained at normal pressure. The tail gas treatment device is one or a combination of two or more of a gas washing bottle, a drying device, and an activated carbon box. A solution for neutralizing or absorbing harmful tail gas is added to the gas washing bottle, a desiccant is added to the drying device, and activated carbon is added to the activated carbon box.

[0022] 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 the receiving 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.

[0023] The principle of the present invention is:

[0024] The present invention achieves precise conveying and continuous preparation of materials with ultra-high airtightness by controlling the external coupling magnet compartment inductively driving the local conveyor belt through a motor, in conjunction with the adjacent and coaxially aligned inner lining cavity material slit, and the feed and receiving silos equipped with buffer bins. The present invention achieves precise conveying and continuous preparation of materials with ultra-high airtightness by combining the confining effect of the inner lining cavity slit with the localized uniform phase pores symmetrically arranged on the inner wall of the central area and the gas barrier formed by the continuously supplied inlet end protective gas. This ensures that each position of the porous bulk material experiences an equally uniform and efficient growth environment during the continuous preparation process. The reaction process is continuous, uniform, and efficient, and significantly breaks through the limitations of material size, especially length.

[0025] The advantages and beneficial effects of the present invention are:

[0026] 1. The present invention proposes a method of continuously and precisely pushing samples in conjunction with a material slit that runs through the axis of the inner lining cavity and has the function of carrying and conveying samples, a reaction gas path that reaches the center of the inner lining cavity, localized uniform-phase air holes that are symmetrically arranged in the middle area of ​​the inner lining cavity (corresponding to the constant temperature zone of the heating furnace body), and a gas barrier effect generated by the continuous supply of protective gas separately arranged at the air inlet end. This ensures that each position of the continuously growing porous bulk 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 material, especially the length of the material. At the same time, the above design, in conjunction with the feed bin and the receiving bin equipped with a buffer bin, realizes the continuity of the material preparation process and the feeding and taking processes.

[0027] 2. This invention utilizes a motor to control an externally coupled magnet compartment to indirectly drive the sample transport mechanism within the device, thus avoiding the need for dynamic sealing interfaces and ensuring 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.

[0028] 3. The present invention proposes to control the conveying device through a programmable motor to ensure the precise control of the feeding, reaction and receiving processes.

[0029] 4. The present invention proposes to use a local conveyor belt to replace the push-pull rod or the belt that runs through the entire reaction chamber. This solution not only avoids the challenges to equipment stability and air tightness caused by the conveyor entering the high-temperature zone, but also breaks through the limitations of the high temperature and complex atmosphere environment in the reaction zone on the conveyor, especially the material of the conveyor belt.

[0030] 5. The present invention proposes a simple and stable structure in which material limit blocks are arranged in an orderly manner on the local conveying crawler. On the one hand, it ensures that the conveying process is one-way transmission, and on the other hand, it ensures that only one sample is pushed each time during the conveying process.

[0031] 6. This invention proposes a uniquely structured inner liner chamber. This utilizes a narrow slit within the inner liner chamber, a localized conveyor belt coaxially aligned with the liner chamber's upper surface, and the inherent transmission of the adjacent bulk material to achieve material loading and conveyance within the high-temperature zone. Because the inner liner chamber remains stationary during operation, temperature and atmosphere disturbances caused by conveyor belts entering the high-temperature reaction zone during the reaction process are avoided.

[0032] 7. The proposed reaction gas path, which directly reaches the center of the liner chamber, and the symmetrically arranged localized uniform-phase pores in the middle region of the reaction chamber (corresponding to the constant-temperature zone of the heating furnace), ensure that the reaction gas does not stratify due to diffusion before reaching the reaction zone, and the localized uniform-phase pores provide a more uniform distribution. Furthermore, a non-uniform design is proposed for the arrangement of the localized uniform-phase pores, with the number of pores gradually increasing from the center to the sides and the aperture gradually expanding. This guides the gas flow and ensures a more uniform atmosphere distribution.

[0033] 8. The present invention proposes to utilize the limiting and guiding effects of the material passing slit and the gas barrier effect generated by the continuous supply of protective gas separately arranged at the air inlet end, so as to cause the reaction atmosphere to be concentrated in the narrow area at the center of the lining cavity to fully contact and penetrate the material, thereby ensuring a more uniform and efficient preparation process.

[0034] 9. Through the above series of improvements and innovations, the present invention provides a continuous, uniform and efficient growth environment for porous bulk materials, significantly improves material quality and production efficiency, greatly reduces production costs, and can play a role in various industries in need. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 . Schematic diagram of the overall structure of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0036] Figure 2 .Schematic diagram of the feeding system structure of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0037] Figure 3 . A cross-sectional view of the feed bin of the feed system of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0038] Figure 4 . Schematic diagram of the reaction system structure of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0039] Figure 5-1 . A cross-sectional view of the gas delivery area of ​​the reaction chamber of the reaction system of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0040] Figure 5-2 A cross-sectional view of the uniform gas reaction zone of the reaction chamber of a reaction system of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials (two-half symmetrical structure).

[0041] Figure 5-3. A cross-sectional view of the reaction chamber track area of ​​a reaction system of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0042] Figure 6-1 .Schematic diagram of the material collection system structure of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0043] Figure 6-2 .Schematic diagram of the material collection system structure of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0044] Figure 7 . A cross-sectional view of the receiving bin of the receiving system of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0045] Figure 8 .Schematic diagram of the gas intake control system structure of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0046] Figure 9 .Schematic diagram of the vacuum system structure of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0047] Figure 10 .Schematic diagram of the exhaust system structure of a chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials.

[0048] In the figure, A is the air intake control system, B is the feeding system, C is the reaction system, D is the receiving system, and E is the exhaust and vacuum system. 1 is the first vacuum pipeline; 2 is the first exhaust pipeline; 3 is the second vacuum pipeline; 4 is the second exhaust pipeline; 5 is the first protective gas pipeline; 6 is the sealing ring cooling jacket; 7 is the radial magnetic coupling coupling; 8 is the driving motor; 9 is the driving gear; 10 is the steering transmission gear; 11 is the fixed bearing; 12 is the material limit block; 13 is the crawler; 14 is the crawler wheel; 15 is the feed bin; 16 is the first door of the feed bin; 17 is the second door of the feed bin; 18 is the observation window; 19 is the bracket; 20 is the push-pull cylinder; 21 is the push-pull cylinder gas line; 22 is the square flexible sealing gasket; 23 is the O-type flexible sealing gasket; 24 is the spiral O-type fastening nut group; 25 is the fastener hole position; 26 is the heating furnace; 27 is the reaction furnace tube; 28 is the reaction chamber gas transmission area; 29 is the reaction Cavity uniform gas reaction zone; 30 reaction chamber track zone; 31 gas transmission pipeline; 32 material limiting track; 33 local uniform phase air hole; 34 reaction gas pipeline; 35 material receiving bin; 36 first-level bin door of material receiving bin; 37 second-level bin door of material receiving bin; 38 material guide plate; 39 gas mixer; 40 mass flow controller; 41 gas circuit valve; 42 vacuum pump; 43 third vacuum pipeline; 44 third tail gas pipeline; 45 second protective gas pipeline; 46 third protective gas pipeline; 47 fourth tail gas pipeline; 48 first check valve; 49 fifth tail gas pipeline; 50 second check valve; 51 gas washing bottle; 52 drying device; 53 activated carbon box; 54 feeding buffer bin; 55 receiving buffer bin; 56 transmission shaft. DETAILED DESCRIPTION

[0049] like Figures 1-10 As shown, the chemical vapor deposition reaction equipment of the present invention, which is suitable for uniform, continuous and efficient preparation of porous macroscopic materials, is composed of an air intake control system A, a feeding system B, a reaction system C, a material collection system D, and an exhaust and vacuum system E. The specific structure is as follows:

[0050] The feed bin 15 of the feed system B is connected to the feed end of the reactor tube 27 of the reaction system C, and the receiving bin 35 of the receiving system D is connected to the discharge end of the reactor tube 27 of the reaction system C; the air intake control system A is connected to the protective gas pipeline interface of the feed system B through the first protective gas pipeline 5, and the air intake control system A is connected to the protective gas pipeline interface of the receiving system D through the second protective gas pipeline 45 and the third protective gas pipeline 46, and the air intake control system A is connected to the reaction gas pipeline interface of the receiving system D through the reaction gas pipeline 34; the vacuum pump 42 of the vacuum system of the tail gas and vacuum system E is connected to the first check valve 48 and then respectively connected to the first vacuum pipeline 1, the second vacuum pipeline 3 and The vacuum pipeline interface of the feeding system B is connected, and the vacuum system of the exhaust gas and vacuum system E is connected to the vacuum pipeline interface of the receiving system D through the third vacuum pipeline 43; the gas washing bottle 51 of the exhaust system of the exhaust gas and vacuum system E is connected to the second check valve 50 and then connected to the exhaust pipeline interface of the feeding system B through the first exhaust pipeline 2 and the second exhaust pipeline 4, and the gas washing bottle 51 of the exhaust system of the exhaust gas and vacuum system E is connected to the second check valve 50 and then connected to the exhaust pipeline interface of the receiving system D through the third exhaust pipeline 44 and / or the fourth exhaust pipeline 47, and the exhaust system of the exhaust gas and vacuum system E is connected to the exhaust pipeline interface of the vacuum system through the fifth exhaust pipeline 49.

[0051] (1) If Figure 8 As shown, the air intake control system A is mainly composed of the following five main parts, namely: gas source, gas circuit valve 41, mass flow controller 40 (or valve plus flow meter combination), gas mixer 39 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 the receiving system D through the gas circuit valve 41, mass flow controller 40, gas mixer 39 and reaction gas pipeline 34. The gas source of protective gas is connected to the protective gas pipeline interface of the feeding system B or the receiving system D through the gas circuit valve 41, mass flow controller 40 and protective gas pipeline (first protective gas pipeline 5, second protective gas pipeline 45, third protective gas pipeline 46). The reaction gas pipeline 34 transports reaction gas to the equipment, and the protective gas pipeline transports protective gas to the equipment.

[0052] Gas valve 41 protects mass flow controller 40 and associated piping by preventing damage caused by prolonged pressure from the gas source. Gas valve 41 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.

[0053] The function of the mass flow controller 40 is to control and adjust the input amount of each gas source.

[0054] The function of the gas mixer 39 is to mix gases, capable of mixing two or more gases simultaneously to prevent excessive stratification in the pipeline. After the gas flow rate is adjusted by a mass flow controller 40 or a valve and flowmeter combination for closed-loop control, the gas is fully mixed and delivered to the reaction chamber of reaction system C through the gas mixer 39. The gas mixer can perform static or dynamic mixing, and its internal structure can be SV, K, SX, SH, SL, SY, or SD type.

[0055] 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.

[0056] (2) If Figure 2-Figure 3 As shown, the feeding system B is mainly composed of the following five main parts, namely: feeding bin 15 (feeding bin first-level bin door 16, feeding bin second-level bin door 17, driving device and sealing gasket), local conveying device (driving motor 8, driving gear 9, steering transmission gear 10, fixed bearing 11, crawler wheel 14, crawler 13 and material limit block 12), observation window 18, sealing ring cooling jacket 6 and bracket 19.

[0057] The feed bin 15 is installed on the bracket 19, and a horizontal feed bin first-level bin door 16 is set at the opening of the upper end thereof. A horizontal feed bin second-level bin door 17 is set below the first-level bin door 16 in the inner cavity of the feed bin 15. The chamber formed between the first-level bin door 16 and the second-level bin door 17 is a feed buffer bin 54. An observation window 18 is installed on one side of the feed bin 15, and a sealing ring cooling jacket 6 is set on the other side of the feed bin 15 at the connection between the feed bin 15 and the feed end of the reaction furnace tube 27 of the reaction system C.

[0058] In the local conveyor, a track 13 mounted on a track wheel 14 is installed within the inner cavity of the feed bin 15, below the secondary bin door 17. Track wheel 14 is powered by a drive motor 8, which transmits power from the outside to the inside via a radial magnetic coupling 7 for sealed transmission. The power is then transmitted to track wheel 14 by main gear 9 via a steering gear pair 10 secured within a fixed bearing 11. One end of a drive shaft 56 passes through the fixed bearing 11 and connects to the steering gear pair 10. The vertical steering gear pair 10 meshes with the horizontal driving gear 9. The output end of the drive motor 8 is connected to the driving gear 9. The steering gear pair 10 is coaxially connected to the center of track wheel 14 via the other end of the drive shaft 56, driving the rotation of track wheel 14. The controllable clockwise / counterclockwise rotation of track wheel 14 drives track 13 forward / reverse at a set speed. Material stoppers 12 are provided on the surface of track 13, distributed over half of the surface.

[0059] The upper flange of the feed bin 15 and the first-level door 16 of the feed bin are sealed by a square flexible sealing gasket 22, and fastener holes 25 are symmetrically opened at the end face of the upper flange of the feed bin 15. The fasteners pass through the first-level door 16 of the feed bin and the upper flange of the feed bin 15 and are installed in the fastener holes 25, so that the first-level door 16 of the feed bin is sealed and connected to the upper flange of the feed bin 15.

[0060] The secondary door 17 of the feed bin is installed in the inner cavity of the feed bin 15 below the primary door 16 of the feed bin in the form of a plug-in plate. The lower ends of the secondary door 17 of the feed bin are sealed with the side walls of the inner cavity of the feed bin 15 by O-type flexible sealing gaskets 23. The upper ends of the secondary door 17 of the feed bin are symmetrically provided with longitudinal push-pull cylinders 20, which are connected to the push-pull cylinder air path 21, and the lifting and lowering of the push-pull cylinder 20 is controlled by the push-pull cylinder air path 21; the outer end of the secondary door 17 of the feed bin is provided with a screw, and the secondary door 17 of the feed bin is connected to the spiral O-type fastening nut group 24 through the screw, and the opening or closing of the secondary door 17 of the feed bin is controlled by the spiral O-type fastening nut group 24.

[0061] The function of the feed bin 15 is to store the materials to be reacted, wherein the first-level bin door 16 of the feed bin seals the entire feed bin 15. When the materials to be reacted need to be replenished, the second-level bin door 17 of the feed bin, the drive device and the sealing gasket work together to isolate and seal the feed buffer bin 54, thereby ensuring that the atmosphere of the reaction system C is not affected by the operation of adding the materials to be reacted.

[0062] The feed bin 15 contains a feed buffer bin 54. The first-level bin door 16 (feed bin door) and the second-level bin door 17 (buffer bin door) of the feed 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 second-level bin door 17 (buffer bin door) of the feed bin is pressurized and sealed and opened and closed in a planar motion by one of the drive devices such as a pull electromagnet, a push electromagnet or a push-pull cylinder. The material of the sealing gasket can be natural rubber, chloroprene rubber, nitrile rubber, fluororubber, chlorosulfonylated polyethylene synthetic rubber, silicone rubber, ethylene propylene rubber, graphite, ceramic fiber, polytetrafluoroethylene or EPDM sponge. The structure of the sealing gasket can be rectangular cross-section, metal winding, flat gasket, corrugated, annular, toothed, triangular, double cone ring, C-shaped or hollow O-shaped.

[0063] The function of the local conveying device is to cooperate with the slit of the inner lining cavity to controllably convey the material to be reacted in the feed bin to the reaction system, wherein the drive motor 8 can be a DC motor, a stepper motor, a servo motor or a combination of a motor and a spindle box transmission, which provides power to the crawler 13 through the active gear 9, the steering transmission gear 10 and the track wheel 14 in sequence. Among them, the material limit block 12 is fixed on the crawler 13 in an orderly manner, and there is a certain gap between the upper surface of the material limit block 12 and the lower surface of the feed bin 15. The function of the material limit block 12 is, on the one hand, to ensure that the conveying process is one-way transmission through the orderly arrangement in the area of ​​the track 13, and on the other hand, to limit the feeding device through simple limiting measures to ensure that only one sample is pushed at a time during the conveying process. Among them, the internal transmission of the feed bin 15 adopts, but is not limited to, the use of gears, screws or direct connections to provide power to the track wheel 14, and the crawler 13 adopts friction transmission or meshing transmission.

[0064] The function of the observation window 18 is to observe the state of the sample at any time, and the function of the sealing ring cooling jacket 6 is to cool the sealing ring to prevent the sealing ring from aging and reducing the airtightness.

[0065] The function of the bracket 19 is to support and fix the feed bin 15 to ensure the stability of the equipment feed bin 15.

[0066] (3) If Figure 4 、 Figure 5-1 、 Figure 5-2 、 Figure 5-3 As shown, the reaction system C is mainly composed of the following three main parts, namely the heating furnace 26, the reaction furnace tube 27 and the lining cavity (the lining cavity is a three-region combination structure, including the reaction chamber gas supply area 28, the reaction chamber uniform gas reaction area 29 and the reaction chamber track area 30). The reaction furnace tube 27 is horizontally arranged in the heating furnace 26. The inner cavity of the reaction furnace tube 27 is sequentially provided with cylindrical reaction chamber gas supply area 28, reaction chamber uniform gas reaction area 29 and reaction chamber track area 30. The outer end of the reaction chamber gas supply area 28 corresponds to the material receiving system D, and the outer end of the reaction chamber track area 30 corresponds to the material feeding system B. The reaction chamber gas supply area 28, the reaction chamber uniform gas reaction area 29 and the reaction chamber track area 30 are arranged in a cylindrical manner. In the middle, a strip-shaped material passing slit is opened in the horizontal direction as a material limiting track 32. The cross-sectional dimensions of the three material limiting tracks 32 are the same and they are interconnected. The material limiting tracks 32 of the reaction chamber gas supply area 28 and the reaction chamber uniform gas reaction area 29 are relatively opened with horizontal gas supply pipelines 31 above and below. Local uniform phase air holes 33 are opened above and below the material limiting tracks 32 of the reaction chamber uniform gas reaction area 29. The middle material passing slit of the lining cavity is coaxially aligned with the local conveying crawler 13 of the feeding system B; the reaction chamber gas supply area 28, the reaction chamber uniform gas reaction area 29 and the reaction chamber track area 30 are connected by threaded connections or straight plug connections, so that the pressurization at the interface can achieve a bevel hard sealing effect.

[0067] The function of the heating furnace 26 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.

[0068] Reactor tube 27 provides a sealed growth chamber for material growth. Its ends connect to feed system B and receiving system D, respectively, and are sealed via flange seals to prevent impurities from entering the system and leaks. Reaction tube 27 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.

[0069] The functions of the liner cavity are as follows: (1) the material to be reacted in the feed bin 15 is controllably conveyed to the reaction system C and finally to the receiving system D through the material passing slit set at its axis and running through the entire liner cavity, and then the local conveying device; (2) the upper and lower gas passages of the reaction chamber gas delivery area 28 are tightly connected to the reaction gas delivery pipeline of the air intake control system A (or in some embodiments, the lower gas passage of the reaction chamber gas delivery area 28 is tightly connected to the reaction gas delivery pipeline, while the upper pipeline is tightly connected to the equipment venting pipeline), and the reaction gas is directly conveyed to the local uniform phase pores 33 in the high temperature reaction zone in the middle of the liner cavity to avoid premature diffusion of the gas and to force the reaction atmosphere to a certain extent in the slit; (3) the reaction chamber uniform gas reaction zone 29 makes the reaction gas uniformly contact or penetrate the material to be reacted through the local uniform phase pores 33 symmetrically set on the upper and lower inner walls of the central area of ​​the liner cavity. In order to make the gas distribution more uniform, the local uniform phase pores 33 gradually become denser from the center to the sides, and the aperture gradually expands, such as Figure 5-2 (4) The inner lining cavity ensures that the reaction gas is confined to a narrow area through the confinement effect of the slit structure and the directional gas delivery, so that the reaction gas is fully in contact with the material, making the preparation process more efficient. The inner lining cavity can be made of metals such as quartz, corundum, boron nitride, silicon carbide, high-strength graphite or stainless steel, preferably graphite or stainless steel.

[0070] (4) If Figure 6-1 、 Figure 6-2 、 Figure 7 As shown, the material receiving system D is mainly composed of the following main parts, namely the material receiving bin 35 (the first-level bin door 36 of the material receiving bin, the second-level bin door 37 of the material receiving bin, the driving device and the sealing gasket), the material guide plate 38, the sealing ring cooling jacket 6 and the bracket 19.

[0071] The material receiving bin 35 is mounted on the bracket 19. A horizontal first-stage bin door 36 is provided at its lower opening. A horizontal second-stage bin door 37 is provided above the first-stage bin door 36 within the inner cavity of the material receiving bin 35. The chamber formed between the first-stage bin door 36 and the second-stage bin door 37 serves as the material receiving buffer bin 55. A sealing ring cooling jacket 6 is provided at the connection between the material receiving bin 35 and the discharge end of the reactor tube 27 of the reaction system C. A material guide plate 38 is provided at the feed end of the material receiving bin 35. Furthermore, a reaction gas line 34 is symmetrically provided on the flange at one end of the material receiving bin 35, or a fourth tail gas line 47 and a reaction gas line 34 are symmetrically provided on the flange at one end of the material receiving bin 35. A protective gas pipeline is provided on the flange at the other end (tail end) of the receiving bin 35. During the reaction process, the protective gas is continuously supplied through the controllable protective gas pipeline to form a gas barrier at the receiving end of the equipment, ensuring that the reaction atmosphere is more locally concentrated in the uniform gas area of ​​the reaction chamber, making the reaction process more efficient.

[0072] The lower end flange of the material receiving bin 35 and the first-level bin door 36 of the material receiving bin are sealed by a square flexible sealing gasket 22, and fastener holes 25 are symmetrically opened at the end face of the lower end flange of the material receiving bin 35. The fasteners pass through the first-level bin door 36 of the material receiving bin and the lower end flange of the material receiving bin 35 and are installed in the fastener holes 25, so that the first-level bin door 36 of the material receiving bin is sealed and connected to the lower end flange of the material receiving bin 35.

[0073] The secondary door 37 of the material receiving bin is installed in the inner cavity of the material receiving bin 35 above the primary door 36 of the material receiving bin in the form of a plug-in plate. The upper two ends of the secondary door 37 of the material receiving bin are sealed with the side walls of the inner cavity of the material receiving bin 35 by an O-type flexible sealing gasket 23. The lower two ends of the secondary door 37 of the material receiving bin are symmetrically arranged with longitudinal push-pull cylinders 20, which are connected to the push-pull cylinder air path 21, and the lifting and lowering of the push-pull cylinder 20 is controlled by the push-pull cylinder air path 21; the outer end of the secondary door 37 of the material receiving bin is provided with a screw, and the secondary door 37 of the material receiving bin is connected to the spiral O-type fastening nut group 24 through the screw, and the opening or closing of the secondary door 37 of the material receiving bin is controlled by the spiral O-type fastening nut group 24.

[0074] The function of the material receiving bin 35 is to store samples after the reaction is completed, wherein the first-level bin door 36 of the material receiving bin seals the entire material receiving bin. When it is necessary to take out the samples after the growth is completed, the second-level bin door, drive device and sealing gasket of the material receiving bin work together to isolate and seal the material receiving buffer bin 55, thereby ensuring that the atmosphere environment of the reaction system is not affected by the operation of taking out the samples after the growth is completed.

[0075] The receiving bin 35 contains a receiving buffer bin 55. The first bin door 36 (receiving bin door) and the second bin door 37 (buffer bin door) of the receiving bin are compressed by fasteners or pressurization to form metal gasket seals, 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 second bin door 37 (buffer bin door) of the receiving bin is pressurized and sealed and opened and closed in a planar motion by one of the drive devices such as a pull electromagnet, a push electromagnet or a push-pull cylinder. The material of the sealing gasket can be natural rubber, chloroprene rubber, nitrile rubber, fluororubber, chlorosulfonylated polyethylene synthetic rubber, silicone rubber, ethylene propylene rubber, graphite, ceramic fiber, polytetrafluoroethylene or EPDM sponge. The structure can be rectangular cross-section, metal winding, flat gasket, corrugated, annular, toothed, triangular, double cone ring, C-shaped or hollow O-shaped.

[0076] The material guide plate 38 regulates the sample's transport motion to prevent stacking and movement, preventing it from reaching the receiving bin. The seal ring cooling jacket 6 cools the seal ring to prevent aging and reduced sealing. The bracket 19 supports and secures the receiving bin 35, ensuring its stability.

[0077] (5) If Figure 9 、 Figure 10 As shown, the exhaust and vacuum system E includes an exhaust system (exhaust treatment device, second check valve 50 and exhaust pipeline, etc.) and a vacuum system (vacuum pump 42, first check valve 48, vacuum pipeline, etc.).

[0078] After the exhaust gas treatment device is connected to the second check valve 50, it is closely connected to the equipment exhaust gas pipeline (first exhaust gas pipeline 2, second exhaust gas pipeline 4, third exhaust gas pipeline 44, fourth exhaust gas pipeline 47, fifth exhaust gas pipeline 49) through the pipeline. When it is turned on, the entire cavity of the equipment or the feed bin / feed buffer bin and the receiving bin / receiving buffer bin are maintained at normal pressure. The exhaust gas treatment device can be one or a combination of two or more of the following: a washing bottle 51 (to which a solution for neutralizing or absorbing harmful exhaust gas can be added), a drying device 52, an activated carbon box 53, etc. An absorption liquid can be added to the washing bottle 51 to neutralize or absorb harmful exhaust gas, a desiccant can be added to the drying device 52, and activated carbon can be added to the activated carbon box 53.

[0079] After connecting to first check valve 48, vacuum pump 42 is tightly connected to the equipment vacuum lines (first vacuum line 1, second vacuum line 3, and third vacuum line 43) 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 the receiving 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, among others.

[0080] 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.

[0081] Example 1

[0082] In the present embodiment, a chemical vapor deposition reaction device suitable for uniform, continuous and efficient preparation of porous macroscopic materials is provided, including: a first vacuum pipeline 1, a first exhaust pipeline 2, a second vacuum pipeline 3, a second exhaust pipeline 4, a first protective gas pipeline 5, a sealing ring cooling jacket 6, a radial magnetic coupling coupling 7, a drive motor 8, an active tooth 9, a steering transmission tooth 10, a fixed bearing 11, a material limit block 12, a crawler 13, a crawler wheel 14, a feed bin 15, a first-level bin door 16 of the feed bin, a second-level bin door 17 of the feed bin, an observation window 18, a bracket 19, a push-pull cylinder 20, a push-pull cylinder gas path 21, a square flexible sealing gasket 22, an O-type flexible sealing gasket 23, a spiral O-type fastening nut group 24, a fastener hole position 25, a heating furnace 26, a reaction furnace tube 27, reaction chamber gas transmission area 28, reaction chamber uniform gas reaction area 29, reaction chamber track area 30, gas transmission pipeline 31, material limiting track 32, local uniform phase air hole 33, reaction gas pipeline 34, material receiving bin 35, material receiving bin first door 36, material receiving bin second door 37, material guide plate 38, gas mixer 39, mass flow controller 40, gas circuit valve 41, vacuum pump 42, third vacuum pipeline 43, third tail gas pipeline 44, second protective gas pipeline 45, third protective gas pipeline 46, fourth tail gas pipeline 47, first check valve 48, fifth tail gas pipeline 49, second check valve 50, gas washing bottle 51, drying device 52, activated carbon box 53, feed buffer bin 54, material receiving buffer bin 55, transmission shaft 56; the specific structure and connection of each component are as follows: Figure 1 、 Figure 2 、 Figure 3 、 Figure 4 、 Figure 5-1 、 Figure 5-2 、 Figure 5-3 、 Figure 6-1 、 Figure 7 、 Figure 8 、 Figure 9 、 Figure 10 shown.

[0083] like Figures 1-10 As shown, the operation process of this embodiment is as follows:

[0084] Adjust the drive motor to transfer the material limit block 12 to the origin (the origin is where the first material limit block just passes over the feed bin 15 and is close to the edge of the reactor tube end), control the push-pull cylinder 20 in the feed bin 15 to make it in a retracted state, loosen the feed bin spiral O-type fastening nut group 24, open the feed bin secondary door 17 horizontally, and tighten the feed bin spiral O-type fastening nut group 24. Take out the fasteners in the feed bin fastener hole 25 and open the feed bin primary door 16. Stack multiple samples to be reacted horizontally in the feed buffer bin 54 (placed on the feed bin secondary door 17), close the feed bin primary door 16, and insert the fasteners into the feed bin fastener hole 25 to tighten and seal the feed bin primary door 16. Close all gas valves in the entire equipment, start the vacuum system pump 42, open the valves of the first vacuum line 1, the second vacuum line 3, and the third vacuum line 43 to remove gas from the feeding system, reaction system C, and receiving system D, close the valves of the first vacuum line 1, the second vacuum line 3, and the third vacuum line 43, and turn off the vacuum system pump 42. Activate the air intake control system A, use the corresponding mass flow controller 40 to control the set shielding gas ventilation flow rate, open the valves of the first shielding gas line 5, the second shielding gas line 45, and the third shielding gas line 46, and after each area is inflated to a positive pressure, close the valves of the first shielding gas line 5, the second shielding gas line 45, and the third shielding gas line 46, and open the valves of the first exhaust gas line 2, the second exhaust gas line 4, and the third exhaust gas line 44 until the air in each area is completely replaced. Close the valves of the second tail gas pipeline 4 and the third tail gas pipeline 44, open the valve of the third protective gas pipeline 46 and continue ventilation, and start the heating furnace 26 to heat the reaction system to the required set temperature. Start the drive motor 8 and run according to the set program (the track 13 moves counterclockwise at a faster set speed. After the material limit blocks 12 are completely separated from the bottom surface of the sample and the material to be reacted completely falls on the plane of the local conveying track 13 without the limit blocks, the local conveying track 13 is controlled to move clockwise at the set speed. The movement distance is the length of the material to be reacted. The material to be reacted is completely conveyed to the reaction chamber track area 30, and the conveying of the material to be reacted is completed once). The set program is repeatedly executed, and the previous piece of material to be reacted is conveyed from the next piece of material to be reacted to the reaction system until the first piece of sample to be reacted is conveyed to the junction of the reaction system track area 30 and the reaction chamber homogenizing reaction area 29. Then the track 13 is controlled to move counterclockwise at a faster set speed. After the material limit blocks 12 are completely separated from the bottom surface of the next piece of material to be reacted and the material to be reacted completely falls on the plane of the local conveying track without the limit blocks, the drive motor 8 is stopped.After the heating furnace 26 reaches the set temperature, the reaction gas flow rate is adjusted and set by the corresponding mass flow controller 40, and the valves of the two reaction gas pipelines 34 symmetrically arranged above and below the flange of the receiving system D are opened. The reaction gas is transported to the reaction chamber uniform gas reaction zone 29 through the reaction chamber gas delivery area 28, and evenly enters the material limiting track 32 in the lining cavity (that is, the lining cavity material passing slit) through the local uniform phase air hole 33. The drive motor 8 is started and continuously operated according to the set program. The local conveyor belt 13 rotates clockwise at the set speed, thereby transmitting the first piece of material through the constant temperature reaction zone at a set speed by the mutual transmission between the materials. After the first piece of material passes through the reaction zone at a uniform speed, the local conveyor belt 13 is controlled by the program to move counterclockwise at a faster set speed. After the material stoppers 12 are completely separated from the bottom surface of the next piece of material to be reacted, and the material to be reacted completely falls on the surface of the local conveyor belt 13 without the stoppers, the local conveyor belt 13 is controlled to rotate clockwise at the set speed (the time delay caused by the counterclockwise rotation of the local conveyor belt when loading the next piece of material can be compensated based on information such as the length of the material to be reacted) to convey the next piece of material into the reaction zone at a uniform speed according to the set growth conditions to complete growth. When the reacted material is transferred to the material receiving system D, the material guide plate 38 adjusts the movement posture of the reacted sample so that it is accurately delivered to the upper surface of the secondary storage door 37 of the material receiving bin 35. When the material to be reacted reaches a certain amount and needs to be taken out, the push-pull cylinder 20 in the receiving bin 35 is controlled to be in a contracted state, the spiral O-type fastening nut group 24 of the receiving bin is loosened, the secondary bin door 37 of the receiving bin is opened horizontally, and the spiral O-type fastening nut group 24 of the receiving bin is tightened. At this time, the material in the receiving bin 35 that has completed the reaction falls into the upper surface of the primary bin door 36 of the receiving bin in the receiving buffer bin 55, the spiral O-type fastening nut group 24 of the receiving bin is loosened, the secondary bin door 37 of the receiving bin is closed horizontally, and the spiral O-type fastening nut group 24 of the receiving bin is tightened. 4. Control the push-pull cylinder 20 in the material receiving bin to extend it, start the vacuum pump 42 of the vacuum system, open the valve of the third vacuum pipeline 43 of the material receiving system, and evacuate the material receiving buffer bin 55. After reaching the required vacuum degree, close the valve of the vacuum pipeline 43 of the material receiving system, close the vacuum pump 42 of the vacuum system, open the valve of the second protective gas pipeline 45 of the material receiving bin to inflate the material receiving buffer bin, and close the second protective gas pipeline 45 after the cabin becomes positive pressure, open the corresponding valve of the third exhaust pipeline 44, and adjust the exhaust device pressure to normal pressure.Take out the fasteners in the fastener hole 25 of the material receiving bin, open the first-level bin door 36 of the material receiving bin, take out the reacted material, close the first-level bin door 36 of the material receiving bin, put the fasteners into the fastener hole 25 of the material receiving bin to tighten and seal, start the vacuum pump 42 of the vacuum system, open the valve of the third vacuum pipeline 43, vacuum the material receiving buffer bin 55, and close the valve of the third vacuum pipeline 43 after reaching the required vacuum degree, turn off the vacuum pump 42 of the vacuum system, open the valve of the second protective gas pipeline 45 of the material receiving bin to inflate the material receiving buffer bin 55, and close the valve of the second protective gas pipeline 45 after the cabin becomes positive pressure, open the corresponding valve of the third exhaust gas pipeline 44, adjust the air pressure of the exhaust device to normal pressure, and then close the valve of the third exhaust gas pipeline 44. When new materials to be reacted need to be added, loosen the spiral O-type fastening nut group 24 of the feed bin, close the secondary bin door 17 of the feed bin horizontally, tighten the spiral O-type fastening nut group 24 of the feed bin, control the push-pull cylinder 20 in the feed bin 15 to make it in an extended state, start the vacuum pump 42 of the vacuum system, open the valve of the second vacuum pipeline 3 of the feed system, and vacuum the feed buffer bin 54. After reaching the required vacuum degree, close the valve of the second vacuum pipeline 3 of the feed system, close the vacuum pump 42 of the vacuum system, open the valve of the feed bin protective gas pipeline 5 to inflate the feed buffer bin, and close the valve of the first protective gas pipeline 5 after the cabin becomes positive pressure, open the corresponding valve of the second exhaust gas pipeline 4, adjust the air pressure of the exhaust device to normal pressure, and then close the valve of the second exhaust gas pipeline 4. Take out the fasteners in the fastener hole 25 of the feed bin, open the first-level bin door 16 of the feed bin, put a certain amount of material to be reacted into the upper surface of the second-level bin door 17 of the feed bin, close the first-level bin door 16 of the feed bin, put the fasteners into the fastener hole 25 of the feed bin for tightening and sealing, start the vacuum pump 42 of the vacuum system, open the valve of the second vacuum pipeline 3 of the feed system, vacuum the feed buffer bin 54, and close the valve of the second vacuum pipeline 3 of the feed system after reaching the required vacuum degree, close the vacuum pump 42 of the vacuum system, open the valve of the first protective gas pipeline 5 of the feed bin to inflate the feed buffer bin 54, and close the valve of the first protective gas pipeline 5 after the cabin becomes positive pressure, open the corresponding valve of the second exhaust gas pipeline 4, adjust the air pressure of the exhaust device to normal pressure, and then close the valve of the second exhaust gas pipeline 4. Control the push-pull cylinder 20 in the feed bin 15 to retract it, loosen the O-ring screw nuts 24, open the secondary door 17 horizontally, and tighten the O-ring nuts 24. The newly added reactant material then falls to the top of the existing reactant material in the feed bin 15. This ensures that the temperature and atmosphere within the reaction system are not affected during the addition and removal process, thus ensuring continuous, uninterrupted growth.

[0085] Example 2

[0086] The equipment structure and most of the operating steps of this embodiment are identical to those of Example 1, with the difference being that, during the reaction in Example 1, the first tail gas line 2 remains open, and the reaction system is maintained at atmospheric pressure. After the heating furnace 26 reaches the set temperature, the first tail gas line 2 is closed during the reaction, and the vacuum pump 42 and first vacuum line 1 are turned on. By adjusting the opening range of the valve in first vacuum line 1 and the flow rates of the reaction gas and shielding gas, the reaction preparation process is achieved under a set negative pressure environment.

[0087] Example 3

[0088] The equipment structure of this embodiment is slightly different from that of embodiment 1. The difference is that the upper pipeline of the reaction gas pipeline 34 symmetrically arranged above and below the flange of the receiving bin in embodiment 1 is replaced by the fourth tail gas pipeline 47 ( Figure 6-2 ), that is, the gas route closely connected to the gas pipeline on the upper side of the reaction chamber gas delivery area is changed from the reaction gas pipeline 34 to the fourth tail gas pipeline 47. For the specific structure and connection of each component, see Figure 1 、 Figure 2 、 Figure 3 、 Figure 4 、 Figure 5-1 、 Figure 5-2 、 Figure 5-3 、 Figure 6-2 、 Figure 7 、 Figure 8 、 Figure 9 、 Figure 10 .

[0089] Most of the operating steps of this embodiment are the same as those of Example 1, with the difference being that in Example 1, the first tail gas pipeline 2 is always open during the reaction process. When the heating furnace reaches the set temperature, the first tail gas pipeline 2 is closed during the reaction process, and the fourth tail gas pipeline 47 is opened. Through the directional drainage effect of the tail gas, the reaction gas is forced to penetrate the porous bulk material to be reacted from bottom to top in the uniform gas zone of the lining cavity, so as to achieve more sufficient and uniform growth of the material in the bulk phase.

[0090] 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, continuous and efficient preparation of porous macroscopic materials, characterized in that: The equipment consists of an air intake control system, a feeding system, a reaction system, a collecting system, and an exhaust and vacuum system. The specific structure is as follows: The feed bin of the feeding system is connected to the feeding end of the reaction furnace tube of the reaction system, and the receiving bin of the receiving system is connected to the discharging end of the reaction furnace tube of the reaction system; the air intake control system is connected to the protection gas pipeline interface of the feeding system through the first protection gas pipeline, the air intake control system is connected to the protection gas pipeline interface of the receiving system through the second protection gas pipeline and the third protection gas pipeline, and the air intake control system is connected to the reaction gas pipeline interface of the receiving system through the reaction gas pipeline; the vacuum system of the tail gas and vacuum system is connected to the vacuum pipeline interface of the feeding system through the first vacuum pipeline and the second vacuum pipeline respectively, and the vacuum system of the tail gas and vacuum system is connected to the vacuum pipeline interface of the receiving system through the third vacuum pipeline; the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface of the feeding system through the first tail gas pipeline and the second tail gas pipeline, the tail gas system of the tail gas and vacuum system is connected to the tail gas pipeline interface of the receiving system through the third tail gas pipeline and / or the fourth tail gas pipeline, 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 fifth tail gas pipeline; The feeding system is provided with a local conveying crawler installed on the crawler wheel. A feeding buffer bin is provided on the upper part of the feeding bin of the feeding system. The slit in the middle of the inner lining cavity of the reaction system is coaxially aligned with the local conveying crawler of the feeding system. A receiving buffer bin is provided on the lower part of the receiving bin of the receiving system. The feed bin of the feeding system is installed on the bracket, and a horizontal first-level feed bin door is provided at the opening of the upper end thereof, and a horizontal second-level feed bin door is provided in the inner cavity of the feed bin below the first-level feed bin door, and the chamber formed between the first-level feed bin door and the second-level feed bin door is a feed buffer bin, an observation window is provided on one side of the feed bin, and a sealing ring cooling jacket is provided on the other side of the feed bin at the connection between the feed bin and the feed end of the reaction furnace tube of the reaction system; a crawler mounted on a track wheel is provided in the inner cavity of the feed bin below the second-level feed bin door, the power of the track wheel is generated by a driving motor, and the power is transmitted from the outside to the inside through a radial magnetic coupling coupling for closed transmission, and the track wheel is powered by gears, screws or direct connections, and the track adopts friction transmission or meshing transmission, and the driving motor is a DC motor, a stepping motor, a servo motor or a combination of a motor and a spindle box transmission; The reaction system includes a heating furnace, a reaction furnace tube and an inner lining cavity. The inner lining cavity is a three-region combination structure, including a reaction chamber gas delivery area, a reaction chamber uniform gas reaction area and a reaction chamber track area. The reaction furnace tube is arranged in the horizontal direction in the heating furnace. The inner cavity of the reaction furnace tube is sequentially provided with a cylindrical reaction chamber gas delivery area, a reaction chamber uniform gas reaction area and a reaction chamber track area. The outer end of the reaction chamber gas delivery area corresponds to the material receiving system, and the outer end of the reaction chamber track area corresponds to the material feeding system. The middle of the reaction chamber gas delivery area, the reaction chamber uniform gas reaction area and the reaction chamber track area are respectively provided with plates in the horizontal direction. The strip-shaped material passing slit serves as a material limiting track. The cross-sectional dimensions of the three material limiting tracks are the same and interconnected. Horizontal gas pipelines are provided above and below the material limiting tracks of the reaction chamber gas supply area and the reaction chamber uniform gas reaction area. Localized uniform phase air holes are provided above and below the material limiting tracks of the reaction chamber uniform gas reaction area, respectively. The arrangement of the localized uniform phase air holes is non-uniform. The number of the localized uniform phase air holes gradually becomes denser from the center to both sides, and the aperture gradually expands. The reaction chamber gas supply area, the reaction chamber uniform gas reaction area and the reaction chamber track area are connected by threaded connections or direct plug-in connections.

2. The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials according to claim 1, characterized in that: The air intake control system includes a gas source, an air 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 receiving system through the air circuit valve, the mass flow controller, the gas mixer, the reaction gas pipeline, and the protective gas pipeline. The gas source of the protective gas is connected to the protective gas pipeline interface of the feeding system or the receiving system through the air 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.

3. The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials according to claim 2, characterized in that: The gas mixer mixes two or more gases simultaneously to prevent excessive stratification of the gases in the pipeline; the gas flow rate is adjusted by the mass flow controller through closed-loop control, and then fully mixed through the gas mixer and transported to the reaction chamber of the reaction system; 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.

4. The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials according to claim 1, characterized in that: The main gear is transmitted to the track wheel through the steering transmission gear fixed in the fixed bearing. One end of the drive shaft passes through the fixed bearing and is connected to the steering transmission gear. The vertical steering transmission gear is engaged with the horizontal active gear. The output end of the drive motor is connected to the active gear. The steering transmission gear is coaxially connected to the center of the track wheel through the other end of the drive shaft to drive the track wheel to rotate. The clockwise / counterclockwise controllable rotation of the track wheel drives the track forward / backward at a set speed; material limit blocks are set on the surface of the track, and the material limit blocks are distributed on half of the track surface.

5. The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials according to claim 1, characterized in that: The first-level door and the second-level door of the feed bin are compressed by fasteners or pressurization to form metal gasket seals, 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 second-level door of the feed bin is pressurized and sealed and opened and closed by a planar motion of a pull electromagnet, a push electromagnet or a push-pull cylinder.

6. The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials according to claim 5, characterized in that: The upper flange of the feed bin and the first-level door of the feed bin are sealed by a square flexible sealing gasket, and the end face of the upper flange of the feed bin is symmetrically opened with fastener holes. The fasteners pass through the first-level door of the feed bin and the upper flange of the feed bin and are installed in the fastener holes, so that the first-level door of the feed bin and the upper flange of the feed bin are sealed and connected; The secondary door of the feed bin is installed in the inner cavity of the feed bin below the primary door of the feed bin in the form of a plug-in plate. The lower ends of the secondary door of the feed bin are sealed with the side walls of the inner cavity of the feed bin by O-type flexible sealing gaskets. The upper ends of the secondary door of the feed bin are symmetrically provided with longitudinal push-pull cylinders, which are connected to the push-pull cylinder air circuit, and the lifting and lowering of the push-pull cylinder is controlled by the push-pull cylinder air circuit; a screw is provided at the outer end of the secondary door of the feed bin, which is connected to the spiral O-type fastening nut group through the screw, and the opening or closing of the secondary door of the feed bin is controlled by the spiral O-type fastening nut group.

7. The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic materials according to claim 1, characterized in that: The receiving bin of the receiving system is installed on the bracket, and a horizontal first-level bin door of the receiving bin is provided at the opening of the lower end thereof, and a horizontal second-level bin door of the receiving bin is provided above the first-level bin door in the inner cavity of the receiving bin, and the chamber formed between the first-level bin door and the second-level bin door of the receiving bin is a receiving buffer bin, and a sealing ring cooling jacket is provided at the connection between the receiving bin and the discharge end of the reaction furnace tube of the reaction system, and a material guide plate is provided at the feed end of the receiving bin; a reaction gas pipeline is symmetrically provided on the flange at one end of the receiving bin, or a fourth tail gas pipeline and a reaction gas pipeline are symmetrically provided on the flange at one end of the receiving bin; a protective gas pipeline is provided on the flange at the other end of the receiving bin, and protective gas is continuously and controllably supplied through the protective gas pipeline during the reaction process to form a gas barrier at the receiving end of the equipment; The lower flange of the receiving bin and the first-level bin door of the receiving bin are sealed by a square flexible sealing gasket, and the end face of the lower flange of the receiving bin is symmetrically opened with fastener holes. The fasteners pass through the first-level bin door of the receiving bin and the lower flange of the receiving bin and are installed in the fastener holes, so that the first-level bin door of the receiving bin is sealed and connected with the lower flange of the receiving bin; The secondary door of the receiving bin is installed in the inner cavity of the receiving bin above the primary door of the receiving bin in the form of a plug-in plate. The upper two ends of the secondary door of the receiving bin are sealed with the side walls of the inner cavity of the receiving bin by O-type flexible sealing gaskets. The lower two ends of the secondary door of the receiving bin are symmetrically arranged with longitudinal push-pull cylinders, which are connected to the push-pull cylinder air circuit, and the lifting and lowering of the push-pull cylinder is controlled by the push-pull cylinder air circuit; a screw is provided at the outer end of the secondary door of the receiving bin, which is connected to the spiral O-type fastening nut group through the screw, and the opening or closing of the secondary door of the receiving bin is controlled by the spiral O-type fastening nut group.

8. The chemical vapor deposition reaction equipment suitable for uniform, continuous and efficient preparation of porous macroscopic 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 equipped with a tail gas treatment device, a second check valve and a tail gas pipeline. The vacuum system is equipped with a vacuum pump, a first check valve and a vacuum pipeline. The specific structure is as follows: 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, the entire cavity of the equipment or the feed bin / feed buffer bin and the receiving bin / receiving buffer bin are maintained at normal pressure. The tail gas treatment device is one or a combination of two or more of a gas washing bottle, a drying device, and an activated carbon box. A solution for neutralizing or absorbing harmful tail gas is added to the gas washing bottle, a desiccant is added to the drying device, and activated carbon is added to the activated carbon box. 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 the receiving 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.

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