CVD (Chemical Vapor Deposition) preparation device and method of graphene material

Abstract

The invention provides a CVD preparation device and method for a graphene material, and relates to the technical field of graphene material preparation. The CVD preparation device of the graphene material comprises a reaction cavity, a vacuum assembly, a gas inlet assembly, a pressure control exhaust assembly and a heating assembly, wherein the reaction cavity is used for accommodating a base material; the vacuum assembly is arranged in the reaction cavity and is communicated with the reaction cavity, and the gas inlet assembly is communicated with one end of the reaction cavity and is used for introducing reaction gas into the reaction cavity; the pressure control exhaust assembly is communicated with the other end of the reaction cavity and is used for exhausting reacted gas and keeping the gas in the reaction cavity to flow stably; the heating assembly is arranged on the outer wall of the reaction cavity, and the heating assembly is configured to move relative to the reaction cavity in the axial direction of the reaction cavity and used for heating the base material, so that graphene grows on the surface of the base material. The heating assembly moves from one end of the base material to the other end of the base material, so that the heater completely traverses the base material in the axial direction of the reaction cavity, and uniform growth of graphene on the base material is realized.

Description

Technical Field

[0001] The present invention generally relates to the technical field of graphene material preparation, and in particular, to a graphene material preparation device and method. Background Art

[0002] Graphene glass fiber fabric is a composite functional material obtained by growing graphene on the surface of a substrate using the method of chemical vapor deposition. The substrate is glass fiber fabric, which is a commonly used engineering material in the fields of engineering, construction, aviation, transportation, energy, and military industry.

[0003] Since the production process of the substrate is mature and the product specifications are stable, the conventional specification is a 1-meter wide coil, and the maximum width can reach 2.6 meters. Existing substrates generally use two methods: the first is to cut the substrate into sheets of a certain length and width, install it on a specific fixture and push it into the process chamber for growth; the second is to cut the coil to a suitable width and install it on a roll-to-roll device for pretreatment and growth. Specifically, after the coil is installed on the unwinding shaft, the free end of the outer layer passes through the process chamber into the winding chamber and is fixed on the winding roller. Using these two methods, there are the following defects:

[0004] 1. In the roll-to-roll growth process, the substrate is laid flat in the process chamber for transmission during the graphene growth process, so that the substrate can only achieve single-layer flat growth. Since the catalytic activity of the glass fiber fabric substrate is relatively low, the growth speed on the substrate is too slow, resulting in a slow transmission speed of the substrate and low growth efficiency;

[0005] 2. The wide substrate is limited by the diameter of the heating furnace and the radial and axial temperature uniformity, so it is impossible to prepare a wide monene glass fiber fabric. Since the width of the substrate is directly limited by the width of the roll-to-roll equipment and the process chamber, it is necessary to increase the width of the process chamber and other dimensions, and the temperature distribution in the width direction of the process chamber is uniform. It is also necessary to increase the investment in other equipment to meet the process capabilities of the high-width roll-to-roll equipment, but the key parameter control of the temperature zone and gas flow field will be more difficult to achieve, and the manufacturing cost will also increase. Summary of the invention

[0006] The present invention provides a CVD preparation device and method for graphene materials, which reduce the limitation of substrate size and improve production efficiency.

[0007] According to a first aspect of the present invention, there is provided a CVD preparation device for graphene material, comprising:

[0008] A reaction chamber, used to accommodate a substrate;

[0009] A vacuum component, connected to the reaction chamber, for extracting air from the reaction chamber;

[0010] An air inlet assembly, connected to one end of the reaction chamber, for introducing reaction gas into the reaction chamber;

[0011] A pressure-controlled exhaust component, connected to the other end of the reaction chamber, for exhausting the reacted gas and maintaining a stable flow of the gas in the reaction chamber;

[0012] A heating component is disposed on the outer wall of the reaction chamber, and the heating component is configured to move along the axial direction of the reaction chamber and relative to the reaction chamber, and is used to heat the reaction chamber so that graphene grows on the surface of the substrate in the reaction chamber.

[0013] In some embodiments, the heating assembly comprises:

[0014] The heater is provided with a central hole, the reaction chamber is penetrated by the central hole, and the reaction chamber and the central hole are slidably matched.

[0015] In some embodiments, the heating assembly further comprises:

[0016] A mobile driving source, wherein an output end of the mobile driving source is connected to the heater, and the mobile driving source drives the heater to move along the axial direction of the reaction chamber;

[0017] A speed control structure is provided on at least one of the mobile driving source and the heater, and is used to adjust the moving speed of the heater.

[0018] In some embodiments, the reaction chamber has a plurality of functional areas along the axial direction of the reaction chamber, and the moving speeds of the heater corresponding to the plurality of functional areas are at least partially different.

[0019] In some embodiments, along the axial direction of the reaction chamber, the length of the heater is L1, the length of the reaction chamber is L, and the length of the substrate is L2;

[0020] Among them, L≥L2+2L1.

[0021] In some embodiments, it also includes:

[0022] An end cover, wherein at least one end of the reaction chamber along the axial direction of the reaction chamber is provided with an open end, and the end cover is sealed at the open end and is detachably connected to the reaction chamber.

[0023] In some embodiments, it also includes:

[0024] A first connecting member, disposed between the end cover and one end of the reaction chamber and detachably connected to the end cover and the reaction chamber respectively;

[0025] Wherein, the air intake assembly is arranged on the first connecting piece, and the air intake assembly is connected with the reaction chamber through the first connecting piece.

[0026] In some embodiments, it also includes:

[0027] A second connecting member is disposed between the end cover and the other end of the reaction chamber and is detachably connected to the end cover and the reaction chamber respectively;

[0028] An exhaust component, disposed on the second connecting piece and connected to the reaction chamber, for exhausting the gas in the reaction chamber;

[0029] A pressure control structure is arranged on the exhaust assembly and is used to maintain the pressure of the reaction chamber.

[0030] In some embodiments, it also includes:

[0031] A vacuum component is disposed on the second connecting piece and communicated with the reaction chamber.

[0032] In some embodiments, the substrate is at least one of a roll structure, a foil, and a sheet structure;

[0033] Alternatively, there are multiple substrates, and the multiple substrates are stacked.

[0034] According to a second aspect of the present invention, an embodiment of the present invention further provides a CVD preparation method of a graphene material, wherein the graphene material is prepared using the CVD preparation device of the graphene material as described above, and the CVD preparation method of the graphene material comprises the following steps:

[0035] placing the substrate in the reaction chamber;

[0036] Connect the end caps to the two ends of the reaction chamber respectively;

[0037] After the reaction chamber is evacuated by the vacuum assembly, a reaction gas is introduced into the reaction chamber by the gas inlet assembly;

[0038] Using a pressure-controlled exhaust component to exhaust the reacted gas and maintain a stable flow of gas in the reaction chamber;

[0039] The heating component is sleeved on the outer wall of the reaction chamber and moves along the axial direction of the reaction chamber and relative to the reaction chamber to heat the reaction chamber and the substrate in the reaction chamber so that graphene grows on the surface of the substrate in the reaction chamber along the movement direction of the heating component.

[0040] An embodiment of the present invention has the following advantages or beneficial effects:

[0041] The embodiment of the present invention provides a CVD preparation device and method for graphene materials, wherein a substrate is placed in a reaction chamber, and a heating component is not fixed relative to the reaction chamber, but is movably arranged relative to the reaction chamber. The heating component can move along the axial direction of the reaction chamber and relative to the reaction chamber, that is, the heating component moves from one end of the substrate to the other end, so that the substrate completely passes through all temperature zones along the axial direction of the reaction chamber, thereby achieving uniform growth of graphene on the substrate. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] In order to better understand the present invention, reference may be made to the embodiments shown in the following drawings. The components in the drawings are not necessarily to scale, and related elements may be omitted in order to emphasize and clearly illustrate the technical features of the present invention. In addition, related elements or components may have different settings as known in the art. In addition, in the drawings, the same reference numerals represent the same or similar components in each of the drawings. The above and other features and advantages of the present invention will become more apparent by describing in detail its exemplary embodiments with reference to the drawings.

[0043] in:

[0044] Figure 1 Shown is a schematic structural diagram of a graphene material preparation device according to an embodiment of the present invention.

[0045] The reference numerals are described as follows:

[0046] 100. Roll structure;

[0047] 1. Reaction chamber; 2. Air inlet assembly; 3. Heating assembly; 4. End cover; 5. First connecting piece; 6. Second connecting piece; 7. Exhaust assembly; 8. Pressure control structure; 9. Vacuum assembly;

[0048] 21. First air intake pipeline; 22. Second air intake pipeline; 23. Third air intake pipeline; 24. Flow detection element; 25. Control valve; 26. Connecting pipeline;

[0049] 31. Heater; 311. Center hole; 32. Mobile driving source; 33. Speed ​​control structure.

[0050] 91. Vacuum pump; 92. Conduit; 93. Vacuum control valve. DETAILED DESCRIPTION

[0051] The following will be combined with the accompanying drawings in the exemplary embodiments of the present invention to clearly and completely describe the technical solutions in the exemplary embodiments of the present invention. The exemplary embodiments described herein are only for illustrative purposes and are not intended to limit the scope of protection of the present invention. Therefore, it should be understood that various modifications and changes can be made to the exemplary embodiments without departing from the scope of protection of the present invention.

[0052] In the description of the present invention, unless otherwise clearly specified and limited, the terms "first" and "second" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance; the term "plurality" refers to two or more; the term "and / or" includes any and all combinations of one or more associated listed items. In particular, reference to "the / the" object or "an" object is also intended to indicate one of a possible plurality of such objects.

[0053] Unless otherwise specified or explained, the terms "connection", "fixation", etc. should be understood in a broad sense. For example, "connection" can be a fixed connection, a detachable connection, an integral connection, an electrical connection, or a signal connection; "connection" can be a direct connection or an indirect connection through an intermediate medium. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0054] Further, in the description of the present invention, it should be understood that the directional words such as "upper", "lower", "inner", "outer" and the like described in the exemplary embodiments of the present invention are described at the angles shown in the accompanying drawings and should not be understood as limiting the exemplary embodiments of the present invention. It should also be understood that, in the context, when it is mentioned that an element or feature is connected to another element (one or more) "upper", "lower", or "inner", "outer", it can not only be directly connected to the other (one or more) elements "upper", "lower", "inner", "outer", but also can be indirectly connected to the other (one or more) elements "upper", "lower", "inner", "outer" through an intermediate element.

[0055] Example embodiments will now be described more fully with reference to the accompanying drawings. However, example embodiments can be implemented in a variety of forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that the present invention will be comprehensive and complete and fully convey the concepts of the example embodiments to those skilled in the art. The same reference numerals in the figures represent the same or similar structures, and thus their detailed description will be omitted.

[0056] The present embodiment provides a graphene material preparation system, which includes a pre-tightening device and a CVD preparation device for graphene material. The pre-tightening device is located outside the CVD preparation device for graphene material. The pre-tightening device is used to wind the substrate into a roll structure 100 so that the gaps between two adjacent layers of the substrate in the roll structure 100 are the same. The CVD preparation device for graphene material is used to prepare graphene on the roll structure 100.

[0057] Specifically, the substrate may be quartz fiber, glass fiber, alumina fiber, silicon carbide fiber, basalt fiber and other fiber braids. For example, the width of the glass fiber fabric is about 0.5 m, 0.7 m, 1 m, 1.4 m and the like.

[0058] The pre-tightening device can be used to roll the substrate in an unfolded state into a roll structure 100, which has the advantages of occupying a small space and being convenient for storage and transportation, and the substrates of the roll structure 100 have the same outer diameter, which is convenient for the subsequent uniform growth of graphene in the roll structure 100. At the same time, during the winding process, a certain torque can be applied to the pre-tightening device, so that the pre-tightening device applies a certain pre-tightening force to the substrate during the process of winding the substrate, and the gaps between two adjacent layers of the substrate in the roll structure 100 are the same, so as to ensure that the tightness of the roll structure 100 is approximately consistent, so as to ensure the uniformity of graphene production.

[0059] This embodiment provides a CVD preparation device for graphene materials, such as Figure 1 As shown, the CVD preparation device of graphene material includes a reaction chamber 1, an air intake assembly 2 and a heating assembly 3. The reaction chamber 1 is used to accommodate a substrate, and the air intake assembly 2 is connected to the reaction chamber 1 and is used to introduce a reaction gas into the reaction chamber 1. The heating assembly 3 is arranged on the outer wall of the reaction chamber 1 and is used to heat the reaction chamber 1 so that graphene grows on the surface of the substrate.

[0060] The reaction chamber 1 has a cylindrical shape, and the reaction chamber 1 may be made of a quartz tube, an alumina tube, or the like.

[0061] It can be understood that the CVD preparation device of graphene materials can be a normal pressure or low pressure chemical vapor deposition system, and the CVD preparation device of graphene materials can also be a microwave plasma chemical vapor deposition system, specifically a normal pressure microwave plasma chemical vapor deposition system or a low pressure microwave plasma chemical vapor deposition system, which can realize the continuous generation of plasma under normal pressure or low pressure.

[0062] Among them, the gas inlet assembly 2 is used to introduce the reaction gas into the reaction chamber 1, and the reaction gas includes an inert gas capable of generating plasma, and the inert gas is selected from one or more of argon, krypton and xenon, and the inert gas flow rate is (10sccm~2000sccm, standard liter per minute); the reaction gas also includes a carbon source gas, and the carbon source gas can be selected from one or more of hydrocarbons, alcohols, ethers, ketones and phenols, wherein the carbon source gas flow rate is 100sccm~2000sccm (sccm, standard milliliters per minute), and the reaction gas also includes an auxiliary gas, and the auxiliary gas can be selected from one or more of hydrogen and carbon dioxide, wherein the auxiliary gas flow rate is 100sccm~5000sccm (sccm, standard milliliters per minute). The concentration of the carbon source affects the discharge stability of the system, and also affects the quality and morphology of graphene, and at the same time affects the production rate of graphene.

[0063] During the gas phase growth of graphene, the power of the microwaves generated by the microwave generating assembly can be adjusted within a range of 200W to 2000W, for example, 700W, 1000W, 2000W, etc. The power of the microwaves affects the quality and morphology of graphene, and also affects the degree of cracking of the carbon source and the conversion rate of the carbon source into graphene.

[0064] When the width of the substrate is relatively large, it is difficult to prepare a wide substrate due to the relatively small size of the existing heating assembly 3, and other structures such as the reaction chamber 1 also need to increase the corresponding size, making it difficult to control key parameters such as the temperature zone and the gas flow field, and the manufacturing cost will increase accordingly. At the same time, the substrate is rolled in and out of the reaction chamber 1 in a roll-to-roll manner, and the substrate can only grow graphene in a single layer in the reaction chamber 1. Due to the low catalytic activity of the glass fiber fabric, the growth rate of the graphene is too slow, resulting in a slow transmission speed of the substrate and low production efficiency.

[0065] To solve this problem, Figure 1 As shown, in the CVD preparation device for graphene material provided in this embodiment, the reaction chamber 1 is used to accommodate the substrate, and the heating component 3 is configured to move along the axial direction of the reaction chamber 1 and relative to the reaction chamber 1, and is used to heat the substrate in the reaction chamber 1 to grow graphene on the surface of the substrate.

[0066] It can be understood that the axial direction of the reaction chamber 1 is the same as or parallel to the axial direction of the roll structure 100. At this time, the width direction of the substrate in the original unfolded state is the length of the roll structure 100 along the axial direction of the reaction chamber 1. The inner diameter of the reaction chamber 1 is greater than or equal to the outer diameter of the roll structure 100, so that the roll structure 100 can be freely placed in the reaction chamber 1 or removed from the reaction chamber 1. The inner diameter of the reaction chamber 1 and the outer diameter of the roll structure 100 can be just matched, so that the roll structure 100 and the reaction chamber 1 are approximately coaxially arranged, and the two can be aligned without other positioning structures.

[0067] The substrate is at least one of a roll structure 100, a strip structure, and a sheet structure; when the substrate is a sheet structure, the substrate may be a foil; or there may be multiple substrates, which are stacked, that is, the multiple substrates are arranged in a regular or irregular order in the reaction chamber 1. This embodiment takes the substrate as a roll structure 100 as an example.

[0068] The CVD preparation device of graphene material provided in this embodiment rolls the substrate into a roll structure 100 and then puts it into the reaction chamber 1. The heating component 3 is not fixed relative to the reaction chamber 1, but is movable relative to the reaction chamber 1. The heating component 3 can move along the axial direction of the reaction chamber 1 and relative to the reaction chamber 1, that is, the heating component 3 moves from one end of the roll structure 100 to the other end, so that the roll structure 100 completely traverses all temperature zones along the axial direction of the reaction chamber 1, and the graphene is uniformly grown on the roll structure 100. At the same time, the method of winding the substrate into the roll structure 100 and moving the heating component 3 is equivalent to growing graphene on multiple layers of substrate at the same time, and the production efficiency is relatively high.

[0069] In one embodiment, the heating assembly 3 includes a heater 31 , the heater 31 is provided with a central hole, the reaction chamber 1 is passed through the central hole, and the reaction chamber 1 and the central hole are slidably matched.

[0070] Since the heater 31 has a center hole, the heater 31 is an annular structure or a cylindrical structure. Before use, the reaction chamber 1 is passed through the center hole of the heater 31, which is equivalent to the heater 31 being arranged around the reaction chamber 1. The heater 31 is used to realize the heating process of the reaction chamber 1 along the circumferential direction of the reaction chamber 1, thereby ensuring the uniformity of the circumferential heating of the roll structure 100. The heater 31 moves along the axial direction of the reaction chamber 1, so that the heater 31 passes through the outer peripheral wall of the entire roll structure 100, ensuring the adequacy of the heating of the roll structure 100. Since the reaction chamber 1 can slide relative to the center hole, the center hole plays a guiding role, improving the smoothness of the movement of the heater 31.

[0071] In one embodiment, along the axial direction of the reaction chamber 1, the length of the heater 31 is L1, the length of the reaction chamber 1 is L, and the length of the substrate is L 2。 Among them, L≥L2+2L1.

[0072] That is, the length of the reaction chamber 1 is as long as possible, the length of the heater 31 is as short as possible, the movable distance of the heater 31 is greater than the total length of the substrate, and as the heater 31 moves along the axial direction of the reaction chamber 1, the heater 31 can fully heat the reaction chamber 1, thereby improving the uniformity of graphene growth on the substrate.

[0073] It is understandable that if the size of the heater 31 remains unchanged, the reaction chamber 1 can be appropriately lengthened; if the size of the reaction chamber 1 remains unchanged, the size of the heater 31 can be appropriately reduced; or the reaction chamber 1 can be lengthened and the length of the heater 31 can be shortened at the same time. As the size of the heater 31 is smaller, a wider glass fiber cloth can be used as a substrate in the same reaction chamber 1, and the uniform growth of graphene can also be ensured.

[0074] In one embodiment, the heating assembly 3 further includes a moving driving source 32 , an output end of the moving driving source 32 is connected to the heater 31 , and the moving driving source 32 drives the heater 31 to move along the axial direction of the reaction chamber 1 .

[0075] In one embodiment, the heating assembly 3 further includes a speed control structure 33 , which is disposed on at least one of the moving driving source 32 and the heater 31 , and is used to limit the moving speed of the heater 31 .

[0076] The speed control structure 33 can be used to limit the moving speed of the heater 31, so that the heater 31 can move at a uniform speed relative to the reaction chamber 1, so as to ensure the uniformity of the growth of graphene on the substrate.

[0077] Among them, the control structure can be a speed controller arranged on the mobile drive source 32, which is used to limit the speed or time of the motor rotation, etc. The speed control structure 33 can also be other structures that can be arranged on the heater 31 and the mobile drive source 32 and have a speed control. Specifically, the speed control structure includes a motor and a lead screw, one end of the lead screw is connected to the motor, and the other end is passed through the threaded hole of the heater 31. At this time, the lead screw and the heater form a lead screw nut pair. The motor drives the lead screw to rotate, and as the lead screw rotates, the heater 31 moves along the axial direction of the lead screw, thereby realizing the movement of the heater.

[0078] Alternatively, the control structure includes a motor, a driving wheel, a driven wheel and a belt, the output end of the motor is connected to the driving wheel, the belt is wound around the driving wheel and the driven wheel, the motor drives the driving wheel to rotate, driving the driven wheel to rotate and the belt to move, and the bottom of the heater 31 is fixed to the belt by a clamping structure, so that the belt drives the heater 31 to move.

[0079] Alternatively, the guide rail trolley of the heater 31 can be self-driven, and the purpose of speed control can be achieved through the motor. As long as the function of speed control can be achieved in this embodiment, its specific structure is not limited.

[0080] In one embodiment, the CVD preparation device of graphene material further includes an end cover 4, and the reaction chamber 1 is provided with an open end at at least one end along the axial direction of the reaction chamber 1, and the end cover 4 is sealed at the open end and is detachably connected to the reaction chamber 1.

[0081] When it is necessary to prepare graphene material, the end cap 4 is removed from the reaction chamber 1 to facilitate the substrate of the rolled structure 100 to enter the interior of the reaction chamber 1 through the open end of the reaction chamber 1, and then the end cap 4 is installed to the open end of the reaction chamber 1 to seal the open end to isolate the external atmosphere and facilitate the growth of graphene in the reaction chamber 1; after the substrate of the rolled structure 100 completes the growth of graphene, the end cap 4 is removed from the reaction chamber 1 to facilitate the roll structure 100 to be removed from the reaction chamber 1 through the open end of the reaction chamber 1.

[0082] The end cover 4 can be used to place the substrate of the roll structure 100 into the reaction chamber 1 or remove it from the reaction chamber 1, which is simpler than the existing roll-to-roll method of transporting the substrate, is convenient to operate, and has a relatively low production cost.

[0083] In one embodiment, the CVD preparation device of graphene material further includes a first connecting member 5, which is disposed between the end cover 4 and one end of the reaction chamber 1 and is detachably connected to the end cover 4 and the reaction chamber 1, respectively.

[0084] Among them, the first connector 5 can be selected as the first flange or other connectors suitable for connecting with the tubular structure. One end of the reaction chamber 1 along its axial direction is connected to the end cover 4 through the first connector 5, and the connection between the end cover 4 and the reaction chamber 1 is realized by the first connector 5. Since the reaction chamber 1 adopts a quartz tube, the end cover 4 can be made of stainless steel with a seal, and the first connector 5 realizes the connection and fixation between the reaction chamber 1 and the end cover 4 of different materials. It can be understood that the first connector 5 and the reaction chamber 1, and the first connector 5 and the end cover 4 can be connected by threaded connection, which is convenient for installation and disassembly.

[0085] In one embodiment, the air intake assembly 2 is disposed on the first connecting member 5 , and the air intake assembly 2 is connected to the reaction chamber 1 through the first connecting member 5 .

[0086] The air intake assembly 2 is integrated into the first connector 5, so that the air intake assembly 2 can deliver air to the reaction chamber 1. The air intake assembly 2 is not directly connected to the reaction chamber 1, so the overall integrity of the reaction chamber 1 will not be damaged. At this time, the first connector 5 not only realizes the intermediate connection between the reaction chamber 1 and the end cover 4, but also provides an installation position for the air intake assembly 2. The first connector 5 realizes functional integration, has multiple uses, and has strong functionality.

[0087] like Figure 1 As shown, the air intake assembly 2 includes a first air intake pipeline 21, a second air intake pipeline 22 and a third air intake pipeline 23. The first air intake pipeline 21 is used to transport a carbon source, the second air intake pipeline 22 is used to transport an auxiliary gas, such as hydrogen, and the third air intake pipeline 23 is used to transport an inert gas, such as argon. The first air intake pipeline 21, the second air intake pipeline 22 and the third air intake pipeline 23 can be directly connected to the air inlet, or connected to the air inlet through a connecting pipeline 26.

[0088] The gas supply pipeline also includes a flow detection component 24, which is specifically a flow detection meter. The flow detection component 24 can be set in at least one of the first air intake pipeline 21, the second air intake pipeline 22 and the third air intake pipeline 23, and is used to detect the gas flow in each air supply pipeline.

[0089] The gas supply pipeline also includes a control valve 25 , which is disposed on the connecting pipeline 26 and is used to control the opening and closing of the connecting pipeline 26 .

[0090] In one embodiment, Figure 1 As shown, the CVD preparation device of graphene material further includes a second connecting member 6, which is disposed between the end cover 4 and the other end of the reaction chamber 1 and is detachably connected to the end cover 4 and the reaction chamber 1 respectively.

[0091] Among them, the second connector 6 can be selected as a second flange or other connectors suitable for connecting with a tubular structure. The other end of the reaction chamber 1 along its axial direction is connected to the end cover 4 through the second connector 6, and the connection between the end cover 4 and the reaction chamber 1 is realized by the second connector 6. Since the reaction chamber 1 adopts a quartz tube, the end cover 4 can be made of stainless steel with a seal, and the second connector 6 realizes the connection and fixation between the reaction chamber 1 and the end cover 4 of different materials. It can be understood that the second connector 6 and the reaction chamber 1, and the second connector 6 and the end cover 4 can be connected by threaded connection, which is convenient for installation and disassembly.

[0092] In one embodiment, the exhaust component 7 is disposed on the second connecting member 6 , and the exhaust component 7 is connected to the reaction chamber 1 through the second connecting member 6 . The exhaust component 7 is used to discharge the gas in the reaction chamber 1 .

[0093] The exhaust assembly 7 is integrated into the second connector 6, so that the exhaust assembly 7 can discharge the exhaust gas in the reaction chamber 1. The exhaust assembly 7 is not directly connected to the reaction chamber 1, so the overall integrity of the reaction chamber 1 will not be damaged. At this time, the second connector 6 not only realizes the middle connection between the reaction chamber 1 and the end cover 4, but also provides an installation position for the exhaust assembly 7. The second connector 6 realizes functional integration, has multiple uses, and has strong functionality.

[0094] In one embodiment, Figure 1 As shown, the CVD preparation device of graphene material further includes a pressure control structure 8 , which is arranged on the exhaust component 7 and is used for maintaining a constant pressure or a stable pressure in the reaction chamber 1 .

[0095] The pressure control structure 8 may be a ball valve or a butterfly valve, and the pressure control structure 8 may be disposed on the exhaust pipe of the exhaust assembly 7. When the pressure control structure 8 is turned on, the gas in the reaction chamber 1 may be directly discharged. Of course, it is understandable that, as the air intake assembly 2 continues to deliver gas to the reaction chamber 1, the valve opening of the pressure control structure 8 may be adjusted at any time according to the change in the air pressure in the reaction chamber 1, so that the air pressure in the reaction chamber 1 remains constant.

[0096] In one embodiment, Figure 1 As shown, the CVD preparation device of graphene material further includes a vacuum component 9 , which is disposed on the second connecting piece 6 and communicated with the reaction chamber 1 .

[0097] Specifically, the vacuum assembly 9 includes a vacuum pump 91, a conduit 92 and a vacuum pressure gauge. One end of the conduit 92 is connected to the vacuum pump 91, and the other end is connected to the second connecting member 6. The vacuum pump 91 is connected to the second connecting member 6 through the conduit 92. Under the vacuum extraction action of the vacuum pump 91, the air in the reaction chamber 1 can be initially extracted, and then the air intake assembly 2 introduces the reaction gas into the reaction chamber 1. A vacuum pressure gauge is also provided on the conduit 92 to detect the vacuum degree in the conduit 92. A vacuum control valve 93 is also provided on the conduit 92 to control the opening and closing of the conduit 92.

[0098] It can be understood that the gas outlet of the second connecting member 6 is connected to two parallel branches, one of which is for directly exhausting the gas in the reaction chamber 1 through the exhaust pipe and the pressure control structure 8. The other branch is connected to the vacuum pump 91 through the conduit 92. When the branch is connected, the reaction chamber 1 is in a low-pressure deposition process.

[0099] This embodiment also provides a CVD preparation method for graphene material, using the above-mentioned CVD preparation device for graphene material to prepare graphene material, and the CVD preparation method for graphene material comprises the following steps:

[0100] Placing the substrate in the reaction chamber 1;

[0101] Connect the end caps 4 to the two ends of the reaction chamber 1 respectively;

[0102] After the reaction chamber 1 is evacuated by the vacuum assembly 9, the reaction gas is introduced into the reaction chamber 1 by the gas inlet assembly 2;

[0103] The heating component 3 is sleeved on the outer wall of the reaction chamber 1 and moves along the axial direction of the reaction chamber 1 and relative to the reaction chamber 1 to heat the reaction chamber 1 and the substrate in the reaction chamber 1 so that graphene grows on the surface of the substrate in the reaction chamber 1 along the moving direction of the heating component 3;

[0104] The pressure-controlled exhaust assembly 7 is used to exhaust the reacted gas and maintain a stable flow of gas in the reaction chamber 1 .

[0105] Specifically, the process of preparing graphene material using the CVD preparation method of graphene material and the CVD preparation device of graphene material is as follows:

[0106] 1. A substrate with a width of about 1 m is rolled into a roll structure 100 with certain inner and outer diameters, and the roll structure 100 is placed in a pretreatment device for surface pretreatment to remove the surface wetting agent or coupling agent so that the original surface of the substrate is exposed.

[0107] 2. Place the pre-treated roll structure 100 into the reaction chamber 1, and connect the two ends of the reaction chamber 1 to the end cap 4 through the first connecting piece 5 and the second connecting piece 6 to ensure air tightness;

[0108] 3. Use the vacuum component 9 to evacuate the vacuum, and heat it to the process temperature, which can be 700° C. to 1100° C., and perform heat preservation treatment, for example, the process temperature can be 1000° C.;

[0109] 4. Open the gas inlet assembly 2, introduce the carbon source gas and set the flow rate of the carbon source gas to 50 sccm to 5000 sccm, for example, the flow rate of methane can be selected to be 300 sccm; introduce hydrogen and set the flow rate of hydrogen to 20 sccm to 5000 sccm, for example, the flow rate of hydrogen can be selected to be 500 sccm, until the pressure rises to the target pressure, the target pressure can be 100 Pa to 5000 Pa, for example, the target pressure can be 1000 Pa;

[0110] 5. The length of the heater 31 is about 20 cm, and the speed of the heater 31 is set. The speed can be set to 5 mm / min to 40 mm / min. For example, the heater 31 moves from one end of the roll structure 100 to the other end at a speed of 5 mm / min and runs at a constant speed for 240 minutes, so that the average surface resistance of the entire roll structure 100 is approximately 1505 Ω / sq.

[0111] Embodiment 2

[0112] This embodiment is similar to the first embodiment, and the only difference is the detailed structure of the reaction chamber 1.

[0113] In the CVD preparation device for graphene material provided in this embodiment, the reaction chamber 1 has multiple functional zones along the axial direction of the reaction chamber 1, and the moving speeds of the heater 31 corresponding to the multiple functional zones are at least partially different.

[0114] That is, the heater 31 does not move at a single speed within the range corresponding to the length of the entire roll-up structure 100 , and different functional areas of the reaction chamber 1 may correspond to different moving speeds to increase the diversity of graphene growth in the roll-up structure 100 .

[0115] This embodiment provides a method for preparing graphene material by CVD and a device for preparing graphene material by CVD. The process of preparing graphene material is as follows:

[0116] 1. A substrate with a width of about 1 m is rolled into a roll structure 100 with certain inner and outer diameters, and the roll structure 100 is placed in a pretreatment device. After surface pretreatment, the surface impregnating agent or coupling agent is removed to expose the original surface of the glass fiber of the substrate.

[0117] 2. Place the pre-treated roll structure 100 into the reaction chamber 1, and connect the two ends of the reaction chamber 1 to the end cap 4 through the first connecting piece 5 and the second connecting piece 6 to ensure air tightness;

[0118] 3. Use the vacuum component 9 to evacuate the vacuum, and heat it to the process temperature, which can be 700° C. to 1100° C., and perform heat preservation treatment, for example, the process temperature can be 1000° C.;

[0119] 4. Open the gas inlet assembly 2, introduce the carbon source gas and set the flow rate of the carbon source gas to 50 sccm to 5000 sccm, for example, the flow rate of methane can be selected to be 300 sccm; introduce hydrogen and set the flow rate of hydrogen to 20 sccm to 5000 sccm, for example, the flow rate of hydrogen can be selected to be 500 sccm, until the pressure rises to the target pressure, the target pressure can be 100 Pa to 5000 Pa, for example, the target pressure can be 1000 Pa;

[0120] 5. The length of the heater 31 is about 20 cm. The speed of the heater 31 is set, and the speed can be set to 5 mm / min to 40 mm / min. For example, in one of the functional areas of the reaction chamber 1, the heater 31 moves at a constant speed of 5 mm / min for 100 min, and then in another functional area of ​​the reaction chamber 1, it moves at a constant speed of 40 mm / min for 12.5 min, so that the roll structure 100 corresponds to the two functional areas, and the average surface resistance of one roll structure 100 is 1533 Ω / sq, and the average surface resistance of the other roll structure 100 is 23462 Ω / sq.

[0121] It should be noted that the embodiments of the present invention are shown in the drawings and described in this specification is only an example of the principle of the present invention. It should be clearly understood by those skilled in the art that the principle of the present invention is not limited to any details or any components of the device shown in the drawings or described in the specification.

[0122] It should be understood that the present invention is not limited in its application to the detailed structure and arrangement of the components proposed in this specification. The present invention can have other embodiments and can be implemented and executed in a variety of ways. The aforementioned variations and modifications fall within the scope of the present invention. It should be understood that the present invention disclosed and defined in this specification extends to all alternative combinations of two or more individual features mentioned or evident in the text and / or the drawings. All these different combinations constitute multiple alternative aspects of the present invention. The embodiments described in this specification illustrate the best mode known for implementing the present invention and will enable those skilled in the art to utilize the present invention.

[0123] Those skilled in the art will readily appreciate other embodiments of the present invention after considering the specification and practicing the invention disclosed herein. The present invention is intended to cover any variations, uses or adaptations of the present invention that follow the general principles of the present invention and include common knowledge or customary techniques in the art that are not disclosed by the present invention. The specification and example embodiments are to be considered exemplary only, and the true scope and spirit of the present invention are indicated by the appended claims.

[0124] It should be understood that the present invention is not limited to the precise structure described above and shown in the drawings, and that various modifications and changes may be made without departing from the scope thereof. The scope of protection of the present invention is limited only by the appended claims.

Claims

1. A CVD preparation device for graphene material, characterized in that: include: A reaction chamber, used for accommodating a substrate; A vacuum component, connected to the reaction chamber, for extracting air from the reaction chamber; An air inlet assembly, connected to one end of the reaction chamber, for introducing reaction gas into the reaction chamber; A pressure-controlled exhaust component, connected to the other end of the reaction chamber, for exhausting the reacted gas and maintaining a stable flow of the gas in the reaction chamber; A heating component is disposed on the outer wall of the reaction chamber, and the heating component is configured to move along the axial direction of the reaction chamber and relative to the reaction chamber, and is used to heat the reaction chamber so that graphene grows on the surface of the substrate in the reaction chamber.

2. The CVD preparation device of graphene material according to claim 1, characterized in that: The heating assembly comprises: A heater, wherein the heater is provided with a central hole, the reaction chamber is provided through the central hole, and the reaction chamber and the central hole are slidably matched; A mobile driving source, wherein an output end of the mobile driving source is connected to the heater, and the mobile driving source drives the heater to move along the axial direction of the reaction chamber; A speed control structure is provided on at least one of the mobile driving source and the heater, and is used to adjust the moving speed of the heater.

3. The CVD preparation device of graphene material according to claim 2, characterized in that: Along the axial direction of the reaction chamber, the reaction chamber has a plurality of functional areas, and the moving speeds of the heater corresponding to the plurality of functional areas are at least partially different.

4. The CVD preparation device of graphene material according to claim 2, characterized in that: Along the axial direction of the reaction chamber, the length of the heater is L1, the length of the reaction chamber is L, and the length of the substrate is L2; Among them, L≥L2+2L1.

5. The CVD preparation device of graphene material according to claim 1, characterized in that: Also includes: An end cover, wherein at least one end of the reaction chamber along the axial direction of the reaction chamber is provided with an open end, and the end cover is sealed at the open end and is detachably connected to the reaction chamber.

6. The CVD preparation device of graphene material according to claim 5, characterized in that: Also includes: A first connecting member, disposed between the end cover and one end of the reaction chamber and detachably connected to the end cover and the reaction chamber respectively; Wherein, the air intake assembly is arranged on the first connecting piece, and the air intake assembly is connected with the reaction chamber through the first connecting piece.

7. The CVD preparation device of graphene material according to claim 5, characterized in that: Also includes: The second connecting member is disposed between the end cover and the other end of the reaction chamber and is detachably connected to the end cover and the reaction chamber respectively.

8. The CVD preparation device of graphene material according to claim 7, characterized in that: The pressure-controlled exhaust assembly comprises: an exhaust component, which is disposed on the second connecting member and communicated with the reaction chamber, and is used to exhaust the gas in the reaction chamber; A pressure control structure is arranged on the exhaust component and is used to maintain the pressure of the reaction chamber.

9. The CVD preparation device of graphene material according to claim 1, characterized in that: The substrate is at least one of a roll structure, a foil structure, and a sheet structure; Alternatively, there are multiple substrates, and the multiple substrates are stacked.

10. A CVD method for preparing graphene material, characterized in that: The graphene material is prepared by using the CVD preparation device of the graphene material according to any one of claims 1 to 9, and the CVD preparation method of the graphene material comprises the following steps: placing a substrate in a reaction chamber; Connect the end caps to the two ends of the reaction chamber respectively; After the reaction chamber is evacuated by the vacuum assembly, a reaction gas is introduced into the reaction chamber by the gas inlet assembly; Using a pressure-controlled exhaust component to exhaust the reacted gas and maintain a stable flow of gas in the reaction chamber; The heating component is sleeved on the outer wall of the reaction chamber and moves along the axial direction of the reaction chamber and relative to the reaction chamber to heat the reaction chamber and the substrate in the reaction chamber so that graphene grows on the surface of the substrate in the reaction chamber along the movement direction of the heating component.

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