Reaction device for graphene growth

Abstract

The invention provides a reaction device for graphene growth. The reaction device comprises a reaction furnace, a crucible, a first shielding assembly, a second shielding assembly and a transmission mechanism, the crucible is arranged in a furnace chamber of the reaction furnace and is used for accommodating a metal catalyst for graphene growth; the first shielding assembly comprises at least two shielding plates, and the at least two shielding plates are arranged at a crucible opening of the crucible at intervals and used for partially covering the crucible opening; the second shielding assembly is stacked above the at least two shielding plates and can at least partially cover a gap between the adjacent shielding plates, and the gap is covered by the second shielding assembly to form a channel for gas replacement in the crucible; the transmission mechanism is in transmission connection with the first shielding assembly and the second shielding assembly and used for driving the first shielding assembly and the second shielding assembly to move till the crucible opening is exposed. According to the reaction device provided by the invention, heat loss in the crucible can be blocked in the heating and melting process of the metal catalyst, so that the heating efficiency is improved, and the energy consumption is reduced.

Description

Technical Field

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

[0002] Compared with the redox method commonly used in the industry, the graphene powder produced by this technology has fewer defects, more controllable number of layers, and better thermal conductivity, and is therefore attracting more and more attention from researchers. When using liquid metal to catalyze the growth of graphene, the metal catalyst must be heated to a molten state before the crucible lid is closed. Therefore, the huge heat radiation from the crucible mouth will inevitably cause a large amount of energy loss. For large-sized crucibles used in large-scale production, a larger crucible mouth will result in more heat energy loss.

[0003] In the prior art, during the heating process, the crucible cover is usually moved down to block heat radiation, and the gas flow rate entering the furnace chamber is reduced as much as possible to reduce the heat energy loss carried by the inert gas when it is discharged. However, since the specific heat capacity of the gas is small and the heat loss is mainly due to heat radiation, reducing the gas flow rate entering the furnace chamber can only reduce part of the heat energy loss; although the downward movement of the crucible cover can block heat radiation to a certain extent, the heat insulation effect is not obvious because the graphite ventilation pipe has good thermal conductivity and most of the crucible mouth area is still not blocked. Summary of the invention

[0004] In view of the above problems in the prior art, the present application provides a reaction device for graphene growth. The specific technical solution is as follows: 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; The crucible is arranged in the furnace chamber of the reaction furnace and is used to accommodate a metal catalyst for graphene growth; The first shielding assembly includes at least two shielding plates, and the at least two shielding plates are arranged at intervals at the crucible opening of the crucible to partially cover the crucible opening; The second shielding assembly is stacked above the at least two shielding plates, and can at least partially cover the interval between the 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 for driving the first shielding assembly and the second shielding assembly to move to expose the crucible opening.

[0005] In a possible implementation manner, the at least two shielding plates include a first shielding plate and a second shielding plate; When the first baffle and the second baffle cover the crucible opening, the first baffle and the second baffle are arranged at intervals, and the interval can expose part of the crucible opening. The outer edges of the first baffle and / or the second baffle extend beyond the outer edge of the crucible opening. The width of the interval between the first baffle and the second baffle is 5-8 cm.

[0006] In a possible implementation, the second shielding assembly includes a third baffle and a fourth baffle, and the orthographic projections of the third baffle and the fourth baffle on the crucible opening can cover the crucible opening.

[0007] In a possible implementation, the baffle includes a stacked expanded graphite layer and a heat insulation layer, and the expanded graphite layer is arranged on the side close to the crucible opening.

[0008] In a possible implementation, the thickness of the expanded graphite layer is 1-3 mm, and the thickness of the heat insulation layer is 15-30 mm.

[0009] In a possible implementation, 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, under the action of the transmission mechanism, the baffle can move in the direction of the transmission mechanism to expose the crucible opening.

[0010] In a possible implementation, the transmission mechanism includes a plurality of transmission components with the same number as the baffle. The transmission components are arranged at intervals in sequence along the circumferential direction of the side wall of the reaction furnace, and the transmission components are in transmission connection with the baffle.

[0011] In a possible implementation, each group of the transmission components includes: A pressure member, which is arranged on the outer wall of the reaction furnace; A moving member, one end of which is movably arranged inside the pressure member, and the other end of the moving member extends into the furnace cavity of the reaction furnace; A traction member, one end of which is connected to the moving member and the other end is connected to the baffle.

[0012] In a possible implementation, the included angle between the traction member and the moving member is 170°-180°.

[0013] In a possible implementation, the reaction device further includes a control device, which is arranged outside the reaction furnace. The control device is connected to the pressure member and is used to control the moving direction and moving speed of the moving member in the pressure member.

[0014] Based on the above technical solution, this application has the following beneficial effects: The reaction device for graphene growth provided in the present application includes a reaction furnace, a crucible, a first shielding component, a second shielding component and a transmission mechanism; the crucible is arranged in the furnace chamber of the reaction furnace, and is used to accommodate a metal catalyst for graphene growth. By arranging the first shielding component and the second shielding component above the crucible mouth, during the heating and melting process of the metal catalyst, the first shielding component and the second shielding component can effectively block the heat radiation, thereby blocking the heat loss in the crucible, shortening the heating and melting time of the metal catalyst, reducing the heating energy consumption, and helping to maintain the high temperature environment in the crucible, ensuring that the metal catalyst is fully melted and maintains a liquid state; a transmission mechanism is arranged that is respectively connected to the first shielding component and the second shielding component for driving the first shielding component and the second shielding component away from the crucible mouth to avoid affecting the descent of the crucible cover and the subsequent reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the technical solutions and advantages in the embodiments of the present application or the prior art, the drawings required for use in the embodiments or the prior art descriptions are briefly introduced below. 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 creative work.

[0016] Figure 1 : A schematic diagram of the structure of a reaction device for graphene growth provided in an embodiment of the present application; 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

[0017] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this application.

[0018] 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 modified by the term "about". The term "about" generally refers to a numerical range that a person of ordinary skill in the art considers to be equivalent to the stated values ​​to produce substantially the same properties, functions, results, etc. A numerical range indicated by a lower value and a higher value is defined to include all numerical values ​​included in the numerical range and all subranges included in the numerical range.

[0019] It should be noted that the terms "first", "second", etc. in the specification and claims of the present application and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the data used in this way can be interchanged where appropriate, so that the embodiments of the present application described herein can be implemented in an order other than those illustrated or described herein. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions.

[0020] The following describes a reaction device for graphene growth provided in an embodiment of the present application. Figure 1 , Figure 1 It is a schematic diagram of the structure of a reaction device for graphene growth. It can be understood that the reaction device structure in the figure is only a technical solution of a specific embodiment of the present application, and the reaction device of the present application may include fewer or more structural features, and is not limited to the device structure described in the figure.

[0021] The reaction device includes 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 component 9 includes at least two shielding plates, and at least two shielding plates are arranged at intervals at the crucible mouth of the crucible 4, and are used to partially cover the crucible mouth; the second shielding component 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 between adjacent shielding plates is covered by the second shielding component 10 to form a channel for gas replacement in the crucible 4; the transmission mechanism is respectively connected to the first shielding component 9 and the second shielding component 10, and is used to drive the first shielding component 9 and the second shielding component 10 to move to expose the crucible mouth. In this way, during the heating process of the metal catalyst, the first shielding component 9 and the second shielding component 10 can shield the crucible mouth, effectively blocking the heat radiation from the crucible mouth, thereby preventing the 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 to detach from the crucible mouth, thereby preventing the shielding component from affecting the lifting and lowering of the crucible cover.

[0022] Specifically, the reaction furnace can be provided with an intake pipe and an outlet pipe for introducing and discharging inert gas, thereby replacing the air inside the reaction furnace and providing an inert atmosphere for the inner cavity of the crucible.

[0023] In some embodiments, at least two baffle plates include a first baffle plate and a second baffle plate; when the first baffle plate and the second baffle plate cover the crucible opening, the first baffle plate and the second baffle plate are spaced apart, and the space between the first baffle plate and the second baffle plate can expose a part of the crucible opening. The outer edges of the first baffle plate and / or the second baffle plate extend beyond the outer edge of the crucible opening. In this way, the first baffle plate and the second baffle plate can cover most of the crucible opening to prevent heat loss from the crucible opening, and the space between the first baffle plate and the second baffle plate can allow the exhaust gas in the crucible 4 to be discharged and exchange gas with the gas outside the crucible 4 through this space.

[0024] Specifically, the width of the space between the first baffle plate and the second baffle plate is 5 - 8 cm. It can be understood that the space between the first baffle plate and the second baffle plate can be any value within 5 - 8 cm, and no enumeration is made here. In this way, if the spacing distance is less than 5 cm, it may cause the gas in the crucible 4 to be unable to be discharged smoothly, resulting in thermal decomposition of the residues in the crucible 4 or the organic components and salts in the metal catalyst during heating, and the by-products generated by thermal decomposition accumulate in the reaction system, thus 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 push open the shielding assembly, affecting the heat insulation effect of the shielding assembly on the crucible opening; if the spacing distance is greater than 8 cm, it will cause the opening area of the crucible opening to be too large, resulting in rapid heat loss and reducing the melting efficiency of the catalyst.

[0025] In other embodiments, at least two baffle plates may include N baffle plates spaced apart, where N is a positive integer greater than 2, and the width of the space between adjacent baffle plates is 5 / (N - 1) - 8 / (N - 1) cm; it can be understood that the width of the space between adjacent baffle plates can be any point value within 5 / (N - 1) - 8 / (N - 1) cm, and no enumeration is made here. In this way, controlling the width of the space between adjacent baffle plates within the above range can effectively block heat loss at the crucible opening while forming a channel for gas exchange at the crucible opening.

[0026] In some embodiments, the second shielding assembly 10 only includes one baffle plate, which can completely cover the space between adjacent baffle plates in the first shielding assembly; or partially cover the space between adjacent baffle plates in the first shielding assembly, and the uncovered space area is 0 - 9 cm 2 ; it can be understood that the uncovered space area can be 0 - 9 cm 2Any point value in it will not be enumerated here. In this way, the air pressure inside and outside the crucible can be balanced, and heat loss caused by too large a gap between the baffle plates can be prevented.

[0027] In some embodiments, the second baffle assembly 10 includes at least a third baffle and a fourth baffle. The orthographic projections of the third baffle and the fourth baffle on the crucible opening can cover the crucible opening. In this way, a single baffle can have a smaller size, which is convenient for the transmission assembly to drive the baffle to quickly disengage from the crucible opening.

[0028] Specifically, the third baffle and the fourth baffle are in contact with each other. The orthographic projections of the third baffle and the fourth baffle on the crucible opening can completely cover the crucible opening, so that while forming a gas replacement channel for the crucible 4 inside between the third baffle and the fourth baffle and the first baffle assembly, it can play a role in blocking heat loss at the crucible opening, which is beneficial to maintaining a high-temperature environment inside the crucible 4.

[0029] Specifically, the outer edges of the third baffle and the fourth baffle extend beyond the outer edge of the crucible opening, and the third baffle and the fourth baffle can completely block the annular plane between the inner wall and the outer wall at the crucible opening. In this way, the centers of gravity of the baffle plates are all located on the annular plane of the crucible opening, which can avoid damage to the expanded graphite layer of the baffle plate caused by heavy pressure; and the annular plane between the inner wall and the outer wall at the crucible opening can be completely blocked, which is beneficial to further improving the heat insulation effect.

[0030] In other embodiments, the third baffle and the fourth baffle are arranged at intervals, and the interval between the third baffle and the fourth baffle can expose part of the interval between the first baffle and the second baffle, forming a ventilation hole directly above the crucible opening; preferably, the area of the ventilation hole is 0 - 9 cm 2 , it can be understood that the area of the ventilation hole can be any point value in 0 - 9 cm 2 , which will not be enumerated here. In this way, while blocking heat loss at the crucible opening, the efficiency of gas replacement between the inside of the crucible 4 and the outside can be increased, exhausting the waste gas generated during the heating process from the crucible 4 and maintaining the pressure balance inside and outside the crucible 4.

[0031] In some embodiments, the baffle plate includes a stacked expanded graphite layer and a heat insulation layer, and the expanded graphite layer is arranged on the side close to the crucible opening. In this way, the expanded graphite layer of the baffle plate contacts the crucible opening plane, which can play a lubricating role, avoiding melting on the surface of the heat insulation layer at high temperature, sticking to the crucible opening plane and the heat insulation layer outside the crucible opening, and avoiding adhesion between the heat insulation layers in the baffle plate, resulting in the transmission mechanism being unable to drive the baffle plate to disengage from the crucible opening; and the expanded graphite plate arranged at the lower layer can effectively prevent the weakening of the strength of the heat insulation material at high temperature and the debris falling into the crucible 4 and polluting the catalyst metal.

[0032] Specifically, the material of the expanded graphite layer includes an expanded graphite plate. The use of the expanded graphite plate is beneficial to improving the flexibility of the shielding plate and preventing the shielding plate from colliding with the reaction furnace 1 after leaving the crucible mouth and causing the shielding plate to break.

[0033] Specifically, the thickness of the expanded graphite layer is 1-3 mm; it is understandable that the thickness of the expanded graphite layer can be any point value in the range of 1-3 mm; illustratively, the thickness of the expanded graphite layer is 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, etc. In this way, the thickness of the expanded graphite sheet is controlled within the above range, and the expanded graphite sheet has a certain structural strength and plays a role in heat insulation. Among them, the length of the expanded graphite sheet is greater than or equal to the outer diameter of the crucible mouth, which can ensure that the crucible mouth can be completely covered after the stacking assembly.

[0034] Specifically, the material of the 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 insulation effect of the baffle plate, so that the baffle plate can effectively block the heat loss in the crucible 4 and greatly shorten the heating time.

[0035] Specifically, the thickness of the heat insulation layer is 15-30 mm; it can be understood that the thickness of the heat insulation layer can be any value between 15-30 mm; illustratively, the thickness of the heat insulation layer is 15 mm, 17 mm, 20 mm, 25 mm, 30 mm, etc. In this way, controlling the thickness of the heat insulation layer within the above range can effectively block the heat loss in the crucible 4 and make the shielding plate have a certain structural strength.

[0036] In some embodiments, the baffle plate has at least a first working state and a second working state. In the first working state, the baffle plate is located above the crucible mouth and can at least partially cover the crucible mouth, so that the baffle plate can effectively block the heat radiation from the crucible mouth; in the second working state, the baffle plate 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.

[0037] In some embodiments, the transmission mechanism includes a plurality of transmission components equal to the number of shielding plates, the transmission components are sequentially arranged at intervals along the circumference of the side wall of the reactor 1, and the transmission components are transmission-connected to the shielding plates. In this way, each shielding plate can be transmission-connected to a different transmission component, so that the movement stroke of each shielding plate can be independently controlled, and each shielding plate can be moved in a time-sharing manner to avoid collision of the shielding plates during movement.

[0038] Preferably, the transmission mechanism includes four sets of transmission components, which are arranged at the same interval along the circumferential direction of the side wall of the reaction furnace 1. The four sets of transmission components are respectively connected to the first baffle, the second baffle, the third baffle and the fourth baffle in a transmission manner, and can drive the four baffles to move in different directions, so as to avoid the collision of the baffles with each other during the process of separating from the crucible 4.

[0039] Specifically, each set of transmission components includes: a pressure member 6, which is arranged on the outer wall of the reaction furnace 1; a moving member 7, one end of which is movably arranged inside the pressure member 6, and the other end of which extends into the furnace cavity of the reaction furnace 1; 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 baffle. In this way, the pressure inside the pressure member can be controlled outside the reaction furnace, and then the movement stroke of the moving member can be controlled. When the crucible 4 is in the state of heating up, the moving member 7 is located at a position close to the crucible opening; when the temperature inside the crucible 4 reaches the preset temperature, the pressure inside the pressure member increases, so that the moving member 7 moves away from the crucible opening, and then drives the baffle away from the crucible opening, and the movement control of the baffle can be realized without affecting the reaction process inside the crucible.

[0040] Exemplarily, the pressure member 6 can be an oil cylinder, and the moving member 7 can be an oil cylinder telescopic rod. One end of the oil cylinder telescopic rod is a movable piston arranged inside the oil cylinder. The oil cylinder drives the telescopic rod to move through positive and negative oil pressures to drive the baffle to move to a position away from the crucible opening. In this way, the multi-stage sleeve structure of the oil cylinder telescopic rod can provide a longer working stroke, so that the oil cylinder can achieve a larger movement range in a limited space, which is convenient for installing other auxiliary devices outside the reaction furnace 1.

[0041] Exemplarily, the traction member 8 can be a traction rope. When the oil cylinder telescopic rod moves, the oil cylinder telescopic rod drives the baffle to move away from the crucible opening through the traction rope; when the baffle completely separates from the crucible opening, the oil cylinder telescopic rod stops moving, and the baffle is suspended in the inner cavity of the reaction furnace through the traction rope.

[0042] In some embodiments, the included angle between the traction member 8 and the moving member 7 is 170°-180°; it can be understood that the included angle between the traction member 8 and the moving member 7 can be any point value within 170°-180°, and no enumeration is made here. In this way, controlling the included angle between the traction member 8 and the moving member 7 within the above range is beneficial to shortening the movement stroke of the moving member 7 and ensuring that the baffle can quickly separate from the crucible opening under the movement state of the moving member 7.

[0043] In some embodiments, the reaction device further includes a first control device, which is disposed outside the reaction furnace 1. The first control device can be connected to the pressure member 6 through the pressure member interface 11, and is used to control the pressure in the pressure member 6, thereby controlling the moving direction and speed of the movable member 7 in the pressure member 6. When the first control device is in the on state, the pressure in 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 shielding plate to move through the traction member 8 until the shielding plate moves to a position that completely exposes the crucible opening. In this way, the pressure member 6 is controlled outside the reaction furnace 1 to realize automatic control of the movement of the shielding plate, and then the shielding plate is separated from the crucible opening without destroying the inert atmosphere environment in the reaction furnace 1, which can avoid the influence of the shielding plate on the descent of the crucible cover, thereby ensuring that the subsequent reaction of graphene growth proceeds smoothly.

[0044] 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 a correspondingly connected motor.

[0045] Specifically, the moving speed of the moving member 7 is 30-50 cm / s; it is understandable that the moving speed of the moving member 7 can be any point value in the range of 30-50 cm / s, which is not enumerated here. If the speed of the moving member 7 is less than 30 cm / s, the shielding plate may not be completely removed from the crucible opening before the crucible cover is lowered, affecting the closing of the crucible cover; if the speed of the moving member 7 is greater than 50 cm / s, the pressure in the pressure member 6 may be too high, causing adverse effects on the pressure member 6.

[0046] 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.

[0047] Specifically, the pressure in the pressure member 6 can be adjusted by the first control device, so that the moving member 7 can move in a direction away from the crucible opening, and the moving member 7 can drive the shielding plate to move through the traction member 8 until the shielding plate moves to a position where the crucible opening is completely exposed. In this way, the movement stroke of the shielding plate in the reaction furnace 1 can be controlled by the external first control device, so as to avoid affecting the inert atmosphere in the reaction furnace 1 and improve the operating convenience of the reaction device.

[0048] 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 to cover the crucible 4, thereby ensuring the smooth progress of subsequent reactions.

[0049] In some embodiments, the reaction device further includes at least one temperature measuring device 5. The temperature measuring device 5 includes a temperature test end and a temperature display end. The temperature test end is in close contact with 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 end can penetrate through the side wall of the reaction furnace 1, facilitating real-time reading of the temperature inside the crucible 4, and is used to determine whether the crucible 4 reaches a preset temperature.

[0050] In some embodiments, a heat insulation layer 3 is sleeved on the outer wall of the crucible 4, and a heat insulating brick is provided at the bottom of the crucible 4. The temperature measuring device 5 can penetrate into the heat insulation layer 3 on the side wall of the crucible 4. The heat insulation layer 3 and the heat insulating brick can be used to block heat loss and ensure that the temperature measuring device 5 accurately detects the actual temperature of the crucible 4. Exemplarily, the heat insulation layer 3 can be a ceramic tube.

[0051] In some embodiments, a movable expanded graphite plate is provided between the first shielding component 9 and the crucible opening, which can prevent the shielding plate from contacting the crucible opening, prevent the surface melt of the heat insulation layer material at the crucible opening from adhering to the bottom of the shielding plate during the heating process, and avoid affecting the smooth detachment of the shielding plate from the crucible opening. 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, causing the metal catalyst therein to melt.

[0052] Exemplarily, the working process of the reaction device for graphene growth provided by the present application is as follows: Place the metal catalyst in the crucible 4, turn on the induction heating device 2, and the inside of the crucible 4 is in a heating state. The first shielding plate and the second shielding plate are spaced above the crucible opening. 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 interval between the first shielding plate and the second shielding plate. The first control device is in the off state, and the moving member 7 of each set of transmission components is in a position close to the crucible opening.

[0053] When the temperature measuring device 5 shows that the temperature inside the crucible 4 reaches the preset temperature, the metal catalyst is in a completely melted state. Turn on the first control device to make the pressure member 6 in a pressurized state, and the moving member 7 moves in a direction away from the crucible opening. The moving member 7 can quickly drive the shielding plate away from the crucible opening through the traction member 8 until the shielding plate completely exposes the crucible opening. When the moving member 7 stops moving, the shielding plate completely detaches from the crucible opening, and the shielding plate can be suspended in the inner cavity of the reaction furnace 1 through the traction member 8.

[0054] 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.

[0055] The specific embodiments of the present application are introduced below in conjunction with the above-mentioned technical scheme. The following examples describe the technical scheme of the present application in more detail, and these examples are only used for illustrative purposes, because it is obvious to those skilled in the art that various modifications and changes are made within the scope of the disclosure of the present application. The reagents used in the examples can be obtained commercially or synthesized according to conventional methods, and can be used directly without further treatment, and the instruments and devices used in the examples can be obtained commercially.

[0056] Example 1 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.

[0057] The first shielding assembly 9 includes a first shielding plate and a second shielding plate, which are used to partially cover 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.

[0058] 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 from 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.

[0059] The transmission mechanism includes four transmission components, which are arranged in sequence along the circumference of the reactor, and the intervals between each transmission component are the same. The four transmission components are respectively connected to the first baffle plate, the second baffle plate, the third baffle plate and the fourth baffle plate. The transmission component includes an oil cylinder, an oil cylinder telescopic rod and a traction rope.

[0060] 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 moving speed of the moving member 7 in the pressure member 6 .

[0061] The reaction device further includes an induction heating device, a heat insulation layer, a second control device, and a temperature measuring device 5. The induction heating device is arranged on the outer wall of the crucible 4, and the heat insulation layer is arranged 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, and the second control device can control the opening and closing of the induction heating device and adjust the heating temperature of the induction heating device. The temperature measuring device 5 includes a temperature test end and a temperature display end. The temperature test end can pass through the induction heating device and the heat insulation layer and be closely attached 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 for real-time reading of the temperature inside the crucible 4.

[0062] This embodiment also provides a method for heating and melting a metal catalyst. Based on the above reaction device for graphene growth, specifically, the method may include the following steps: Add 100 kg of copper into the crucible 4, set the first shielding component 9 and the second shielding component 10 above the crucible opening, turn on the induction heating device through the second control device, and set the heating power of the induction heating device to 40 KW; Test the temperature of the crucible through the temperature measuring device 5. When the temperature of the crucible reaches 1300 °C, turn on the first control device to increase the pressure in the oil cylinder. The oil cylinder telescopic rod drives the baffle plate away from the crucible opening, and controls the closing of the crucible cover through the lifting device.

[0063] Record that the heating-up time of the crucible from room temperature to 1300 °C is 70 min.

[0064] Comparative Example 1 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. In the state where the crucible cover is not closed, set the heating power to 40 KW, and record that the heating-up time of the crucible from room temperature to 1300 °C is 150 min. Since no shielding component is provided at the crucible opening, a large amount of heat radiation will be generated at the crucible opening during the heating-up process, resulting in a large amount of energy consumption loss, and increasing the time required for the crucible to be heated to the preset temperature.

[0065] Comparative Example 2 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. A graphite gas pipe integrally connected to the crucible cover is provided. The distance between the pipe orifice of the graphite gas pipe 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 lowered state, the heating power is set to 40 KW, and the heating-up time for the crucible to be heated from room temperature to 1300 °C is recorded as 130 min. Since the crucible cover is in the lowered state, it can block part of the thermal radiation. However, due to the good thermal conductivity of the graphite gas pipe and most areas of the crucible orifice still not being shielded, the heat insulation effect is not obvious. Compared with Example 1, the time required for the crucible to be heated to the preset temperature increases.

[0066] Comparative Example 3 The difference between this comparative example and Example 1 is that in this comparative example, the third baffle and the fourth baffle are arranged at intervals, and the interval between the third baffle and the fourth baffle can expose part of the interval between the first baffle and the second baffle, forming a ventilation hole directly above the crucible orifice, and the area of the ventilation hole is 12 cm 2 . The heating power is set to 40 KW, and the heating-up time for the crucible to be heated from room temperature to 1300 °C is recorded as 85 min. Since the area of the ventilation hole is relatively large, it fails to effectively block the thermal radiation. Compared with Example 1, the time required for the crucible to be heated to the preset temperature increases.

[0067] In summary, it shows that the reaction device provided in this application, by arranging the first shielding component and the second shielding component above the crucible orifice, can effectively block the thermal radiation of the crucible orifice during the heating and melting process of the metal catalyst, reduce the energy loss during the heating process, and thus shorten the heating time.

[0068] The above description has fully disclosed the specific implementation manners of this application. It should be noted that any changes made by those skilled in the art to the specific implementation manners of this application do not depart from the scope of the claims of this application. Correspondingly, the scope of the claims of this application is not limited solely to the foregoing specific implementation manners.

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, the at least two shielding plates being arranged at intervals at the crucible opening of the crucible (4) and being used to partially cover the crucible opening; The second shielding assembly (10) is stacked above the at least two shielding plates and is capable of at least partially covering the interval between adjacent shielding plates, the interval being covered by the second shielding assembly (10) to form a channel for gas replacement in the crucible (4); 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.

2. The reaction device according to claim 1, wherein 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 an interval, and the interval can expose a portion 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; the interval width between the first shielding plate and the second shielding plate is 5-8cm.

3. The reaction device according to claim 1, wherein 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 are capable of covering the crucible opening.

4. The reaction device according to any one of claims 1 to 3, characterized in that, The shielding plate comprises an expanded graphite layer and a heat insulation layer which are stacked, 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, wherein 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 move 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 1-3, characterized in that, The transmission mechanism comprises a plurality of transmission components, the number of which is the same as the number of the shielding plates, the transmission components being arranged in sequence and spaced apart along the circumference of the side wall of the reaction furnace (1), and the transmission components 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 arranged 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 of the traction member (8) 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 includes a first control device, which is arranged outside the reaction furnace (1). The first control device is connected to the pressure member (6) and is used to control the moving direction and moving speed of the moving member (7) in the pressure member (6).

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