A reaction device for graphene growth

Abstract

The present application provides a reaction device for graphene growth, comprising a reaction furnace, a crucible, a first shielding assembly, a second shielding assembly, and a transmission mechanism; the crucible is disposed in the furnace chamber of the reaction furnace, and is used to accommodate a metal catalyst for graphene growth; the first shielding assembly comprises at least two shielding plates, and the at least two shielding plates are spaced apart and disposed at the crucible opening of the crucible, and are used to partially cover the crucible opening; the second shielding assembly is stacked above the at least two shielding plates, and is capable of at least partially covering the interval between adjacent shielding plates, and the interval is covered by the second shielding assembly to form a channel for gas replacement in the crucible; the transmission mechanism is respectively connected to the first shielding assembly and the second shielding assembly, and is used to drive the first shielding assembly and the second shielding assembly to move to expose the crucible opening. The reaction device provided by the present application can block heat loss in the crucible during the heating and melting of the metal catalyst, which is beneficial to improving heating efficiency and reducing energy consumption.

Description

Technical Field

[0001] The present application relates to the field of carbon material technology, and in particular to a reaction device for graphene growth. Background Art

[0002] Liquid metal-catalyzed graphene powder growth is attracting increasing research interest due to its ability to produce graphene with fewer defects, more controllable layer numbers, and superior thermal conductivity compared to the commonly used redox method. However, when growing graphene using liquid metal catalysis, the metal catalyst must be heated to a molten state before the crucible lid is closed. Consequently, the significant heat radiation from the crucible mouth inevitably results in significant energy losses. For large crucibles used in large-scale production, the larger crucible mouth results in even greater heat loss.

[0003] Existing techniques typically lower the crucible lid during the heating process to block heat radiation and minimize the gas flow rate into the furnace chamber to reduce heat energy loss carried by the inert gas when it is exhausted. However, because the specific heat capacity of gas is small and heat loss is primarily due to thermal radiation, reducing the gas flow rate into the furnace chamber only partially reduces heat energy loss. While lowering the crucible lid can block heat radiation to a certain extent, the insulation effect is not significant due to the high thermal conductivity of the graphite ventilation pipe and the fact that most of the crucible opening remains exposed. Summary of the Invention

[0004] In response to the above-mentioned problems in the prior art, the present application provides a reaction device for graphene growth. The specific technical solution is as follows:

[0005] The present application provides a reaction device for graphene growth, the reaction device comprising a reaction furnace, a crucible, a first shielding component, a second shielding component and a transmission mechanism;

[0006] The crucible is arranged in the furnace chamber of the reaction furnace and is used to accommodate the metal catalyst for graphene growth;

[0007] The first shielding assembly includes at least two shielding plates, and the at least two shielding plates are spaced apart and arranged at the crucible opening of the crucible to partially cover the crucible opening;

[0008] The second shielding assembly is stacked above the at least two shielding plates and can at least partially cover the gap between adjacent shielding plates, wherein the gap is covered by the second shielding assembly to form a channel for gas replacement in the crucible;

[0009] The transmission mechanism is respectively connected to the first shielding assembly and the second shielding assembly for driving the first shielding assembly and the second shielding assembly to move to expose the crucible opening.

[0010] In a possible implementation manner, the at least two shielding plates include a first shielding plate and a second shielding plate;

[0011] When the first shielding plate and the second shielding plate cover the crucible mouth, the first shielding plate and the second shielding plate are arranged at intervals, and the intervals can expose part of the crucible mouth, and the outer edges of the first shielding plate and / or the second shielding plate exceed the outer edge of the crucible mouth; the width of the interval between the first shielding plate and the second shielding plate is 5-8 cm.

[0012] In a possible implementation manner, the second shielding assembly includes a third shielding plate and a fourth shielding plate, and the orthographic projections of the third shielding plate and the fourth shielding plate on the crucible opening can cover the crucible opening.

[0013] In a possible implementation manner, the shielding plate includes an expanded graphite layer and a heat insulation layer that are stacked, and the expanded graphite layer is arranged on a side close to the crucible opening.

[0014] In a possible implementation manner, the expanded graphite layer has a thickness of 1-3 mm, and the thermal insulation layer has a thickness of 15-30 mm.

[0015] In a possible embodiment, the baffle has at least a first working state and a second working state. In the first working state, the baffle is located above the crucible opening and can at least partially cover the crucible opening; in the second working state, the baffle can move toward the direction of the transmission mechanism under the action of the transmission mechanism to expose the crucible opening.

[0016] In a possible implementation manner, the transmission mechanism includes a plurality of transmission assemblies, the number of which is the same as the number of the shielding plates, and the transmission assemblies are sequentially spaced along the circumference of the side wall of the reactor, and the transmission assemblies are in transmission connection with the shielding plates.

[0017] In a possible implementation manner, each group of the transmission components includes:

[0018] A pressure piece, the pressure piece being arranged on the outer wall of the reaction furnace;

[0019] a moving member, one end of which is movably disposed inside the pressure member, and the other end of which extends into the furnace chamber of the reaction furnace;

[0020] A traction member, one end of which is connected to the moving member, and the other end of which is connected to the shielding plate.

[0021] In a possible implementation manner, the angle between the traction member and the moving member is 170°-180°.

[0022] In a possible implementation manner, the reaction device further includes a control device, which is disposed outside the reaction furnace and connected to the pressure member, for controlling the moving direction and speed of the moving member in the pressure member.

[0023] Based on the above technical solution, this application has the following beneficial effects:

[0024] The reaction device for graphene growth provided in the present application includes a reactor, a crucible, a first shielding assembly, a second shielding assembly and a transmission mechanism; the crucible is arranged in the furnace chamber of the reactor for accommodating a metal catalyst for graphene growth, and by arranging the first shielding assembly and the second shielding assembly above the crucible mouth, during the heating and melting process of the metal catalyst, the first shielding assembly and the second shielding assembly can effectively block heat radiation, thereby blocking heat loss in the crucible, shortening the heating and melting time of the metal catalyst, reducing heating energy consumption, and helping to maintain a high-temperature environment in the crucible, ensuring that the metal catalyst is fully melted and maintains a liquid state; a transmission mechanism is provided, which is respectively connected to the first shielding assembly and the second shielding assembly for driving the first shielding assembly and the second shielding assembly away from the crucible mouth to avoid affecting the descent of the crucible cover and the subsequent reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the technical solutions and advantages of the embodiments of the present application or the prior art, the following is a brief introduction to the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0026] Figure 1 : A schematic structural diagram of a reaction device for graphene growth provided in an embodiment of the present application;

[0027] Figure numerals: 1-reaction furnace, 2-induction heating device, 3-insulation layer, 4-crucible, 5-temperature measuring device, 6-pressure piece, 7-moving piece, 8-traction piece, 9-first shielding assembly, 10-second shielding assembly, 11-pressure piece interface. DETAILED DESCRIPTION

[0028] The following will be combined with the accompanying drawings in the embodiments of this application to clearly and completely describe the technical solutions in the embodiments of this application. Obviously, the embodiments described are only part of the embodiments of this application, not all of the embodiments. Based on the embodiments of this application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.

[0029] For the following defined terms, these definitions shall apply unless a different definition is given in the claims or elsewhere in this specification. All numerical values, whether or not explicitly indicated, are defined herein as being modified by the term "about". The term "about" generally refers to a numerical range that one of ordinary skill in the art would consider equivalent to the stated value to produce substantially the same properties, functions, results, etc. A numerical range indicated by a lower value and an upper value is defined to include all numerical values ​​included in the numerical range and all subranges included in the numerical range.

[0030] It should be noted that the terms "first," "second," and the like in the specification and claims of this application and the accompanying drawings are used to distinguish similar objects and are not necessarily used to describe a particular order or precedence. It should be understood that the terms used in this manner are interchangeable where appropriate, so that the embodiments of the present application described herein can be implemented in an order other than that illustrated or described herein. In addition, the terms "including," "having," and any variations thereof are intended to cover non-exclusive inclusions.

[0031] The following describes a reaction device for graphene growth provided by the embodiment of the present application. Figure 1 , Figure 1 This is a schematic diagram of the structure of a reaction device for graphene growth. It is understood that the reaction device structure in the figure is only a technical solution of a specific embodiment of the present application. The reaction device of the present application may include fewer or more structural features and is not limited to the device structure depicted in the figure.

[0032] The reaction device includes a reactor 1, a crucible 4, a first shielding assembly 9, a second shielding assembly 10 and a transmission mechanism; the crucible 4 is arranged in the furnace chamber of the reactor 1, and is used to accommodate a metal catalyst for graphene growth; the first shielding assembly 9 includes at least two shielding plates, and at least two shielding plates are spaced apart at the crucible mouth of the crucible 4, and are used to partially cover the crucible mouth; the second shielding assembly 10 is stacked above the at least two shielding plates, and can at least partially cover the gap between adjacent shielding plates. After the gap between adjacent shielding plates is covered by the second shielding assembly 10, a channel for gas replacement in the crucible 4 is formed; the transmission mechanism is respectively connected to the first shielding assembly 9 and the second shielding assembly 10, and is used to drive the first shielding assembly 9 and the second shielding assembly 10 to move to expose the crucible mouth. In this way, during the heating process of the metal catalyst, the crucible mouth can be shielded by the first shielding component 9 and the second shielding component 10, effectively blocking the heat radiation from the crucible mouth, thereby preventing heat loss in the crucible 4; and by providing a transmission mechanism connected to the shielding component, when the temperature in the crucible 4 reaches a preset temperature, the operation of the transmission mechanism can be controlled to drive the shielding component away from the crucible mouth, thereby preventing the shielding component from affecting the lifting and lowering of the crucible cover.

[0033] Specifically, the reaction furnace may be provided with an air inlet pipe and an air outlet pipe for introducing and exhausting inert gas, thereby replacing the air in the reaction furnace and providing an inert atmosphere for the inner cavity of the crucible.

[0034] In some embodiments, at least two shielding plates include a first shielding plate and a second shielding plate; when the first shielding plate and the second shielding plate cover the crucible mouth, the first shielding plate and the second shielding plate are spaced apart, and the space between the first shielding plate and the second shielding plate can expose part of the crucible mouth, and the outer edge of the first shielding plate and / or the second shielding plate exceeds the outer edge of the crucible mouth. In this way, the first shielding plate and the second shielding plate can cover most of the crucible mouth to prevent heat loss from the crucible mouth, and the space between the first shielding plate and the second shielding plate can allow the exhaust gas in the crucible 4 to be discharged and exchanged with the gas outside the crucible 4 through the space.

[0035] Specifically, the spacing width between the first shielding plate and the second shielding plate is 5-8 cm. It is understandable that the spacing between the first shielding plate and the second shielding plate can be any value between 5-8 cm, which is not enumerated here. In this way, if the spacing distance is less than 5 cm, the gas in the crucible 4 may not be discharged smoothly, causing the residue in the crucible 4 or the organic components and salts in the metal catalyst to undergo thermal decomposition during the heating process, causing the by-products generated by the thermal decomposition to accumulate in the reaction system, thereby affecting the quality of the subsequently grown graphene; and the gas cannot be discharged in time, which may cause the internal pressure of the crucible 4 to increase, and the shielding component will be pushed open, affecting the heat insulation effect of the shielding component on the crucible mouth; if the spacing distance is greater than 8 cm, the crucible mouth opening area will be too large, which will cause the heat to dissipate rapidly and reduce the melting efficiency of the catalyst.

[0036] In other implementations, the at least two shielding plates may include N shielding plates spaced apart, where N is a positive integer greater than 2, and the spacing between adjacent shielding plates is 5 / (N-1)-8 / (N-1) cm. It is understood that the spacing between adjacent shielding plates can be any value between 5 / (N-1)-8 / (N-1) cm, which is not enumerated here. Thus, controlling the spacing between adjacent shielding plates within the aforementioned range effectively prevents heat loss from the crucible opening while forming a channel at the crucible opening for gas exchange.

[0037] In some embodiments, the second shielding assembly 10 includes only one shielding plate, which can completely cover the gap between adjacent shielding plates in the first shielding assembly; or partially cover the gap between adjacent shielding plates in the first shielding assembly, and the uncovered gap area is 0-9 cm 2 It is understood that the uncovered interval area can be 0-9cm 2In this way, the pressure inside and outside the crucible can be kept balanced, and heat loss caused by excessive spacing between the shielding plates can be prevented.

[0038] In some embodiments, the second shielding assembly 10 includes at least a third shielding plate and a fourth shielding plate, and the orthographic projections of the third shielding plate and the fourth shielding plate on the crucible mouth can cover the crucible mouth. In this way, a single shielding plate can have a smaller size, making it easier for the transmission assembly to drive the shielding plate to quickly detach from the crucible mouth.

[0039] Specifically, the third shielding plate and the fourth shielding plate offset each other, and the orthographic projections of the third shielding plate and the fourth shielding plate on the crucible mouth can completely cover the crucible mouth, so that the third shielding plate and the fourth shielding plate form a gas replacement channel in the crucible 4 between themselves and the first shielding component, while also playing a role in blocking heat loss from the crucible mouth, which is conducive to maintaining a high temperature environment in the crucible 4.

[0040] Specifically, the outer edges of the third baffle plate and the fourth baffle plate extend beyond the outer edge of the crucible mouth, and the third baffle plate and the fourth baffle plate can completely block the annular plane between the inner wall and the outer wall at the crucible mouth. In this way, the center of gravity of the baffle plate is located on the annular plane of the crucible mouth, which can avoid damage to the expanded graphite layer of the baffle plate due to heavy pressure; and the annular plane between the inner wall and the outer wall at the crucible mouth can be completely blocked, which is conducive to further improving the thermal insulation effect.

[0041] In some other embodiments, the third shielding plate and the fourth shielding plate are spaced apart, and the space between the third shielding plate and the fourth shielding plate can expose part of the space between the first shielding plate and the second shielding plate, forming an air vent just above the crucible opening; preferably, the area of ​​the air vent is 0-9 cm 2 It is understood that the area of ​​the vent holes can be 0-9cm 2 In this way, while blocking the heat loss at the crucible mouth, the efficiency of gas replacement between the inside and outside of the crucible 4 is increased, the waste gas generated during the heating process is discharged from the crucible 4, and the pressure inside and outside the crucible 4 is kept balanced.

[0042] In some embodiments, the shielding plate includes a laminated expanded graphite layer and a thermal insulation layer, with the expanded graphite layer positioned on the side closest to the crucible opening. This allows the expanded graphite layer of the shielding plate to contact the crucible opening plane, providing lubrication and preventing the thermal insulation layer from melting during high temperatures and adhering to the crucible opening plane and the thermal insulation layer outside the crucible opening. It also prevents the individual thermal insulation layers within the shielding plate from adhering to each other, potentially preventing the transmission mechanism from driving the shielding plate away from the crucible opening. Furthermore, the placement of the expanded graphite plate as the lower layer effectively prevents the thermal insulation material from weakening at high temperatures, allowing debris to fall into the crucible 4 and contaminate the catalyst metal.

[0043] Specifically, the material of the expanded graphite layer includes expanded graphite plates. The use of expanded graphite plates is beneficial to improving the flexibility of the shielding plate and preventing the shielding plate from colliding with the reactor 1 after leaving the crucible port and causing the shielding plate to break.

[0044] Specifically, the expanded graphite layer has a thickness of 1-3 mm. It is understood that the thickness of the expanded graphite layer can be any value within this range; illustratively, the thickness of the expanded graphite layer is 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, etc. By controlling the thickness of the expanded graphite sheet within this range, the expanded graphite sheet possesses a certain structural strength while also providing thermal insulation. The length of the expanded graphite sheet is greater than or equal to the outer diameter of the crucible opening, ensuring that the crucible opening is completely covered after stacking and assembly.

[0045] Specifically, the material of the thermal insulation layer includes at least one of high-temperature resistant ceramic fiber felt, asbestos felt, aerogel fiber felt, carbon felt and glass fiber felt, which can effectively improve the thermal insulation effect of the baffle, so that the baffle can effectively block the heat loss in the crucible 4 and greatly shorten the heating time.

[0046] Specifically, the thickness of the thermal insulation layer is 15-30 mm. It is understood that the thickness of the thermal insulation layer can be any value within the range. For example, the thickness of the thermal insulation layer is 15 mm, 17 mm, 20 mm, 25 mm, 30 mm, etc. By controlling the thickness of the thermal insulation layer within the aforementioned range, heat loss within the crucible 4 can be effectively blocked, while also providing the shielding plate with a certain structural strength.

[0047] In some embodiments, the baffle has at least a first working state and a second working state. In the first working state, the baffle is located above the crucible mouth and can at least partially cover the crucible mouth, so that the baffle can effectively block the heat radiation from the crucible mouth; in the second working state, the baffle can move toward the direction of the transmission mechanism under the action of the transmission mechanism to expose the crucible mouth, so as to avoid affecting the descent of the crucible cover and the progress of subsequent reactions.

[0048] In some embodiments, the transmission mechanism includes a plurality of transmission assemblies, equal in number to the number of shielding plates. The transmission assemblies are sequentially spaced along the circumference of the sidewall of the reactor 1 and are in driving connection with the shielding plates. This allows each shielding plate to be connected to a different transmission assembly, enabling independent control of its travel and enabling time-sharing movement of each shielding plate to prevent collisions during movement.

[0049] Preferably, the transmission mechanism includes four groups of transmission components, which are arranged at the same distance along the circumference of the side wall of the reactor 1. The four groups of transmission components are respectively connected to the first baffle plate, the second baffle plate, the third baffle plate and the fourth baffle plate, and can drive the four baffle plates to move in different directions to avoid the baffle plates colliding with each other in the process of separating from the crucible 4.

[0050] Specifically, each transmission assembly includes: a pressure member 6, which is disposed on the outer wall of the reactor 1; a moving member 7, one end of which is movably disposed inside the pressure member 6, and the other end of which extends into the furnace chamber of the reactor 1; and a traction member 8, one end of which is connected to the moving member 7 and the other end of which is connected to the shielding plate. In this way, the pressure inside the pressure member can be controlled outside the reactor, thereby controlling the movement stroke of the moving member. When the crucible 4 is heated, the moving member 7 is located near the crucible opening. When the temperature inside the crucible 4 reaches a preset temperature, the pressure inside the pressure member increases, causing the moving member 7 to move away from the crucible opening, thereby driving the shielding plate away from the crucible opening. This allows the movement of the shielding plate to be controlled without affecting the reaction process inside the crucible.

[0051] For example, the pressure member 6 can be a cylinder, and the movable member 7 can be a telescopic rod of the cylinder. One end of the telescopic rod is a movable piston disposed within the cylinder. The cylinder drives the telescopic rod through forward and reverse oil pressure, thereby moving the shielding plate to a position away from the crucible opening. In this way, the multi-stage sleeve structure of the telescopic rod of the cylinder can provide a longer working stroke, allowing the cylinder to achieve a larger range of motion within a limited space, facilitating the installation of other auxiliary devices outside the reactor 1.

[0052] Exemplarily, the traction member 8 can be a traction rope. When the cylinder telescopic rod is moving, the cylinder telescopic rod drives the baffle to move away from the crucible mouth through the traction rope; when the baffle is completely separated from the crucible mouth, the cylinder telescopic rod stops moving, and the baffle is suspended in the inner cavity of the reactor through the traction rope.

[0053] In some embodiments, the angle between the pulling member 8 and the moving member 7 is 170°-180°. It is understood that the angle between the pulling member 8 and the moving member 7 can be any value between 170°-180°, which is not enumerated here. Thus, controlling the angle between the pulling member 8 and the moving member 7 within the aforementioned range helps shorten the travel of the moving member 7 and ensures that the shielding plate can quickly disengage from the crucible opening when the moving member 7 is in motion.

[0054] In some embodiments, the reaction device further includes a first control device, which is disposed outside the reactor 1. The first control device can be connected to the pressure member 6 via the pressure member interface 11, and is used to control the pressure within the pressure member 6, thereby controlling the direction and speed of movement of the movable member 7 within the pressure member 6. When the first control device is in an on state, the pressure within the pressure member 6 increases, and the movable member 7 can move in a direction away from the crucible opening. The movable member 7 can drive the baffle to move via the traction member 8 until the baffle moves to a position where the crucible opening is completely exposed. In this way, the pressure member 6 is controlled outside the reactor 1 to automatically control the movement of the baffle, thereby separating the baffle from the crucible opening without destroying the inert atmosphere within the reactor 1. This can avoid the influence of the baffle on the descent of the crucible cover, thereby ensuring that the subsequent reactions of graphene growth proceed smoothly.

[0055] Preferably, the first control device comprises a plurality of motors having the same number as the transmission components, each motor being used to control a group of transmission components, so that each shielding plate can be individually controlled by the corresponding connected motor.

[0056] Specifically, the moving member 7 has a moving speed of 30-50 cm / s. It is understood that the moving member 7 can have any value within this range, which is not enumerated here. If the moving member 7 has a speed less than 30 cm / s, the shielding plate may not be completely removed from the crucible opening before the crucible lid is lowered, affecting the closing of the crucible lid. If the moving member 7 has a speed greater than 50 cm / s, excessive pressure may be generated in the pressure member 6, adversely affecting the pressure member 6.

[0057] Preferably, the moving member 7 moves in the pressurizing member in an ejection manner, which can shorten the movement stroke of the moving member 7 in the pressurizing member and achieve the effect of quickly driving the shielding plate away from the crucible opening.

[0058] Specifically, the first control device can adjust the pressure within the pressure member 6, causing the movable member 7 to move away from the crucible opening. The movable member 7 can then drive the shielding plate through the pulling member 8 until the shielding plate moves to a position that completely exposes the crucible opening. In this way, the movement of the shielding plate within the reactor 1 can be controlled by the external first control device, avoiding affecting the inert atmosphere within the reactor 1 and facilitating improved operational convenience of the reactor.

[0059] In some embodiments, the reaction device also includes a crucible cover and a lifting device. The crucible cover can fit tightly with the crucible 4. The lifting device is transmission-connected to the crucible cover and is used to control the lifting and lowering movement of the crucible cover relative to the crucible 4. When the temperature in the crucible 4 reaches a preset temperature, the crucible cover can be driven to move and cover the crucible 4, thereby ensuring the smooth progress of subsequent reactions.

[0060] In some embodiments, the reaction device also includes at least one temperature measuring device 5, which includes a temperature testing end and a temperature display end. The temperature testing end is close to the side wall of the crucible 4 and can accurately detect the actual temperature of the corresponding position of the crucible 4; the temperature display end can pass through the side wall of the reaction furnace 1, which is convenient for real-time reading of the temperature inside the crucible 4, and is used to determine whether the crucible 4 reaches the preset temperature.

[0061] In some embodiments, an insulation layer 3 is provided on the outer wall of the crucible 4, and insulation bricks are provided on the bottom of the crucible 4. The temperature measuring device 5 can penetrate from the insulation layer 3 on the side wall of the crucible 4. The insulation layer 3 and the insulation bricks can be used to block heat loss and ensure that the temperature measuring device 5 accurately detects the actual temperature of the crucible 4; illustratively, the insulation layer 3 can be a ceramic tube.

[0062] In some embodiments, a movable expanded graphite plate is provided between the first shielding assembly 9 and the crucible mouth, which can prevent the shielding plate from contacting the crucible mouth, prevent the surface melt of the insulation layer material at the crucible mouth from adhering to the bottom of the shielding plate during the heating process, and avoid affecting the shielding plate from smoothly detaching from the crucible mouth.

[0063] In some embodiments, the reaction device further includes an induction heating device 2 and a second control device. The induction heating device 2 is arranged on the outer wall of the crucible 4. The second control device is electrically connected to the induction heating device 2. The second control device can control the opening and closing of the induction heating device 2 and adjust the heating temperature of the induction heating device 2 to heat the crucible 4 until the temperature inside the crucible 4 reaches a preset temperature, so that the metal catalyst therein is melted.

[0064] Illustratively, the working process of the reaction device for graphene growth provided in the present application is: a metal catalyst is placed in a crucible 4, the induction heating device 2 is turned on, the crucible 4 is in a heated state, the first shielding plate and the second shielding plate are spaced apart above the crucible mouth, the third shielding plate and the fourth shielding plate are abutted and stacked above the first shielding plate and the second shielding plate, and can at least partially cover the gap between the first shielding plate and the second shielding plate; the first control device is in a closed state, and the moving parts 7 of each group of transmission assemblies are in a position close to the crucible mouth.

[0065] When the temperature measuring device 5 indicates that the temperature inside the crucible 4 has reached a preset temperature, indicating that the metal catalyst is completely melted, the first control device is activated, causing the pressure member 6 to be pressurized, and the movable member 7 to move away from the crucible opening. The movable member 7, via the pulling member 8, can rapidly drive the shielding plate away from the crucible opening until the shielding plate fully exposes the crucible opening. When the movable member 7 stops moving, the shielding plate is completely separated from the crucible opening and can be suspended within the inner cavity of the reactor 1 via the pulling member 8.

[0066] In this way, during the heating and melting process of the metal catalyst, the first shielding component and the second shielding component can effectively block thermal radiation, thereby blocking heat loss in the crucible, shortening the heating and melting time of the metal catalyst, and reducing heating energy consumption; when the temperature in the crucible 4 reaches the preset temperature, the shielding plate can be driven away from the crucible mouth through the transmission mechanism to avoid affecting the descent of the crucible cover and the subsequent reaction.

[0067] The following describes specific embodiments of the present application in conjunction with the above-mentioned technical solutions. The following examples describe the technical solutions of the present application in more detail. These examples are intended for illustrative purposes only, as various modifications and variations within the scope of the present disclosure will be apparent to those skilled in the art. The reagents used in the examples are commercially available or synthesized according to conventional methods and can be used directly without further processing. The instruments and devices used in the examples are all commercially available.

[0068] Example 1

[0069] refer to Figure 1 This embodiment provides a reaction device for graphene growth, including a reaction furnace, a crucible 4, a first shielding component 9, a second shielding component 10 and a transmission mechanism; the crucible 4 is arranged in the furnace chamber of the reaction furnace for accommodating a metal catalyst for graphene growth.

[0070] The first shielding assembly 9 includes a first shielding plate and a second shielding plate for partially covering the crucible opening. The first shielding plate and the second shielding plate are spaced apart at the crucible opening of the crucible 4, and the spacing between the first shielding plate and the second shielding plate is 5-8 cm.

[0071] The second shielding assembly 10 is stacked above the first shielding plate and the second shielding plate. The second shielding assembly 10 includes a third shielding plate and a fourth shielding plate. The third shielding plate and the fourth shielding plate are offset against each other and can completely cover the gap between the first shielding plate and the second shielding plate. The gap between the first shielding plate and the second shielding plate is covered by the second shielding assembly 10 to form a channel for gas replacement in the crucible 4.

[0072] The transmission mechanism includes four transmission assemblies, spaced circumferentially along the reactor, with equal spacing between each assembly. The four transmission assemblies are respectively connected to the first, second, third, and fourth shielding plates. The transmission assemblies include a hydraulic cylinder, a telescopic rod, and a traction rope.

[0073] The reaction device further comprises a first control device arranged outside the reaction furnace, the first control device being connected to the pressure member 6 via the pressure member interface 11 and being used for controlling the moving direction and speed of the moving member 7 in the pressure member 6 .

[0074] The reaction device also includes an induction heating device, an insulation layer, a second control device, and a temperature measuring device 5. The induction heating device is disposed on the outer wall of the crucible 4, and the insulation layer is disposed between the induction heating device and the outer wall of the crucible 4. The induction heating device is electrically connected to the second control device, which can control the induction heating device to turn on and off and adjust the heating temperature of the induction heating device. The temperature measuring device 5 includes a temperature testing terminal and a temperature display terminal. The temperature testing terminal can pass through the induction heating device and the insulation layer to closely contact the side wall of the crucible 4, and can accurately detect the actual temperature at the corresponding position of the crucible 4; the temperature display terminal can penetrate the side wall of the reactor and is used to read the temperature inside the crucible 4 in real time.

[0075] This embodiment further provides a method for heating and melting a metal catalyst, based on the above-mentioned reaction device for graphene growth. Specifically, the method may include the following steps:

[0076] 100 kg of copper was added to the crucible 4, and the first shielding assembly 9 and the second shielding assembly 10 were placed above the crucible opening. The induction heating device was turned on by the second control device, and the heating power of the induction heating device was set to 40 kW.

[0077] The crucible temperature is tested by the temperature measuring device 5. When the crucible temperature reaches 1300°C, the first control device is turned on to increase the pressure in the oil cylinder. The oil cylinder telescopic rod drives the shielding plate to separate from the crucible mouth, and the lifting device is used to control the closing of the crucible cover.

[0078] The crucible was heated from room temperature to 1300°C for 70 minutes.

[0079] Comparative Example 1

[0080] This comparative example differs from Example 1 in that the reaction apparatus provided in this comparative example does not include the first shielding assembly 9, the second shielding assembly 10, or the transmission mechanism. With the crucible lid uncovered, the heating power was set to 40 kW, and the crucible was heated from room temperature to 1300°C in 150 minutes. Because the crucible opening lacks a shielding assembly, significant heat radiation is generated from the opening during the heating process, resulting in significant energy loss and increased time required to heat the crucible to the preset temperature.

[0081] Comparative Example 2

[0082] The difference between this comparative example and Example 1 is that the reaction device provided in this comparative example does not include the first shielding component 9, the second shielding component 10 and the transmission mechanism, and a graphite vent tube integrally connected to the crucible cover is provided. The distance between the nozzle of the graphite vent tube and the metal catalyst at the bottom of the crucible is greater than or equal to 5 cm. When the crucible cover is in the downward position, the heating power is set to 40 kW, and the heating time of the crucible from room temperature to 1300°C is recorded as 130 minutes. Since the crucible cover is in the downward position, it can block some heat radiation. However, due to the good thermal conductivity of the graphite vent tube and the fact that most areas of the crucible mouth are still not blocked, the insulation effect is not obvious. Compared with Example 1, the time required to heat the crucible to the preset temperature is increased.

[0083] Comparative Example 3

[0084] The difference between this comparative example and Example 1 is that in this comparative example, the third shielding plate and the fourth shielding plate are spaced apart, and the gap between the third shielding plate and the fourth shielding plate can expose part of the gap between the first shielding plate and the second shielding plate, forming an air vent just above the crucible mouth, and the area of ​​the air vent is 12 cm 2 The heating power was set to 40 kW, and the crucible was heated from room temperature to 1300°C in 85 minutes. Due to the large area of ​​the vent holes, heat radiation was not effectively blocked. Compared to Example 1, the time required to heat the crucible to the preset temperature increased.

[0085] In summary, the reaction device provided in the present application, by arranging a first shielding component and a second shielding component above the crucible mouth, can effectively block the heat radiation from the crucible mouth during the heating and melting process of the metal catalyst, reduce the energy loss during the heating process, and thus shorten the heating time.

[0086] The above description has fully disclosed the specific embodiments of this application. It should be noted that any changes made by those skilled in the art to the specific embodiments of this application do not depart from the scope of the claims of this application. Accordingly, the scope of the claims of this application is not limited to the above specific embodiments.

Claims

1. A reaction device for graphene growth, characterized in that: The reaction device comprises a reaction furnace (1), a crucible (4), a first shielding component (9), a second shielding component (10) and a transmission mechanism; The crucible (4) is arranged in the furnace chamber of the reaction furnace (1) and is used to accommodate a metal catalyst for graphene growth; The first shielding assembly (9) comprises at least two shielding plates, and the at least two shielding plates are arranged at intervals at the crucible opening of the crucible (4) and are used to partially cover the crucible opening; The second shielding assembly (10) is stacked above the at least two shielding plates and can at least partially cover the interval between adjacent shielding plates, and the interval is covered by the second shielding assembly (10) to form a channel for gas replacement in the crucible (4); the orthographic projection of the second shielding assembly (10) at the crucible opening can cover the crucible opening; The transmission mechanism is respectively connected to the first shielding assembly (9) and the second shielding assembly (10) for driving the first shielding assembly (9) and the second shielding assembly (10) to move to expose the crucible opening; the transmission mechanism includes a traction member (8); when the shielding plate is completely separated from the crucible opening, the shielding plate is suspended in the furnace chamber of the reaction furnace (1) through the traction member (8).

2. The reaction device according to claim 1, characterized in that The at least two shielding plates include a first shielding plate and a second shielding plate; When the first shielding plate and the second shielding plate cover the crucible mouth, the first shielding plate and the second shielding plate are arranged at intervals, and the intervals can expose part of the crucible mouth, and the outer edges of the first shielding plate and / or the second shielding plate exceed the outer edge of the crucible mouth; the width of the interval between the first shielding plate and the second shielding plate is 5-8 cm.

3. The reaction device according to claim 1, characterized in that The second shielding assembly (10) comprises a third shielding plate and a fourth shielding plate, and the orthographic projections of the third shielding plate and the fourth shielding plate on the crucible opening can cover the crucible opening.

4. The reaction device according to any one of claims 1 to 3, characterized in that The shielding plate includes an expanded graphite layer and a heat insulation layer which are stacked together, and the expanded graphite layer is arranged on a side close to the crucible opening.

5. The reaction device according to claim 4, characterized in that The thickness of the expanded graphite layer is 1-3 mm, and the thickness of the heat insulation layer is 15-30 mm.

6. The reaction device according to claim 4, characterized in that The shielding plate has at least a first working state and a second working state. In the first working state, the shielding plate is located above the crucible opening and can at least partially cover the crucible opening; In the second working state, the shielding plate can be moved toward the transmission mechanism to expose the crucible opening under the action of the transmission mechanism.

7. The reaction device according to any one of claims 1 to 3, characterized in that The transmission mechanism comprises a plurality of transmission assemblies, the number of which is the same as the number of the shielding plates, the transmission assemblies being arranged in sequence and spaced apart along the circumference of the side wall of the reaction furnace (1), and the transmission assemblies being in transmission connection with the shielding plates.

8. The reaction device according to claim 7, characterized in that Each group of transmission components includes: A pressure piece (6), the pressure piece (6) being arranged on the outer wall of the reaction furnace (1); a moving member (7), one end of the moving member (7) being movably disposed inside the pressure member (6), and the other end of the moving member (7) extending into the furnace chamber of the reaction furnace (1); A traction member (8), one end of the traction member (8) is connected to the moving member (7), and the other end is connected to the shielding plate.

9. The reaction device according to claim 8, characterized in that The included angle between the traction member (8) and the moving member (7) is 170°-180°.

10. The reaction device according to claim 8, characterized in that The reaction device further comprises a first control device, which is arranged outside the reaction furnace (1) and is connected to the pressure member (6) for controlling the moving direction and moving speed of the moving member (7) in the pressure member (6).

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