CN219991731U - Function expansion part of bubble CVD equipment and graphene film growth device - Google Patents
Function expansion part of bubble CVD equipment and graphene film growth device Download PDFInfo
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- CN219991731U CN219991731U CN202321074957.1U CN202321074957U CN219991731U CN 219991731 U CN219991731 U CN 219991731U CN 202321074957 U CN202321074957 U CN 202321074957U CN 219991731 U CN219991731 U CN 219991731U
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Abstract
The utility model discloses a function expansion part of bubble CVD equipment and a graphene film growth device, and relates to the technical fields of graphene growth preparation and production equipment design, wherein the function expansion part comprises the following characteristics: (1) The whole part consists of an upper disc, a middle disc, a lower disc, a central uniform gas column and an isolation sealing column; (2) The modularized design is adopted, so that the installation, the disassembly and the maintenance are easy; (3) The component is combined with the characteristics of BCVD equipment, and can be used for preparing metal and nonmetal-based high-quality graphene films. The design of the component innovatively expands the functions of the bubble CVD equipment, so that the function of the bubble CVD equipment is diversified, and besides the original preparation of powder, the production and the preparation of 16 graphene films with the size of 4 inches can be provided at a time in the current effective growth space.
Description
Technical Field
The utility model relates to the technical field of graphene growth preparation and production equipment design, in particular to a function expansion part of a bubble CVD (chemical vapor deposition) device and a graphene film growth device.
Background
Graphene is a carbon atom in sp 2 The hybridized single-layer carbon atom two-dimensional material is successfully prepared from 2004 until now, and has excellent physical and chemical properties such as electric conduction, heat conduction, high mechanical strength and the like, so that the material becomes a key material for promoting future technological progress. Among the numerous synthetic methods of graphene materials, a Chemical Vapor Deposition (CVD) method is recognized as a method for preparing high-quality graphene, which can prepare high-quality, large-size, single-crystal and ultra-clean graphene films on various substrates through a proper ratio of hydrocarbon gas sources at a certain growth temperature.
The CVD method is extended with a Bubble CVD (BCVD) method, which is a preparation technology capable of realizing the production of high-quality large-scale graphene powder, and mainly comprises the steps of dispersing and introducing a carbon-containing precursor into molten copper liquid to form bubbles with adjustable sizes, providing a bubble cavity for the growth of graphene, forming graphene on the inner surface of the bubble cavity, carrying the graphene to the surface of the copper liquid along with the rising-burst of the bubbles in the copper liquid, and finally carrying the graphene out of a reaction chamber by air flow disturbance and collecting the graphene. The BCVD method expands the product form of the traditional CVD graphene from a single film form to a powder form, and also has higher quality.
At present, BCVD graphene powder is mainly produced and prepared by means of a pre-designed BCVD device (CN 202110832518.1), wherein the device comprises a sealed cavity, and a heating device for heating copper to a molten state is arranged in the cavity; the cavity is connected with an air inlet device, and the air inlet device is used for introducing the hydrocarbon mixed gas into the heating device; one side of the cavity is connected with a collecting device, and the collecting device is used for collecting graphene; the cavity is also connected with a cooling device for cooling the gas mixture generated by the reaction. As innovative graphene powder production equipment, the graphene powder production equipment has the characteristics of normal pressure growth environment, large-range variable air supply rate, high temperature rise and reduction rate, capability of realizing industrial production and the like. However, the problem of single function exists in the use process, namely, only powder production can be performed, the advantages of a mild growth pressure environment, a rapid temperature rise and reduction process, cold wall equipment characteristics, industrial production capacity and the like of the powder cannot be fully utilized, and thus, idle waste of equipment resources is easily caused, and the additional cost of products is high.
Disclosure of Invention
Aiming at the problems of the prior art, the utility model designs the function expansion part of the bubble CVD equipment and the graphene film growing device, and the function expansion part for the BCVD can grow and prepare the 4-inch metal and nonmetal substrate graphene film by combining the characteristics of rapid temperature rise and reduction, large growth cavity, normal pressure growth and industrial production capacity of the BCVD equipment, so that the equipment function is expanded.
The utility model provides a function expansion part of bubble CVD equipment, which is positioned in a cavity of the bubble CVD equipment and comprises an upper disc, a lower disc, a central gas homogenizing column and an isolation sealing column;
the upper disc is provided with a hollow separation cabin structure, the upper side of each cabin is close to the upper part of the cavity of the bubble CVD equipment, and the lower side of each cabin is provided with a plurality of air outlet sieve holes for air outflow; the lower disc is arranged in parallel corresponding to the lower side of the upper disc and is used for loading a growth substrate;
the upper end of the central air homogenizing column is communicated and fixed with a corresponding interface of the bubble CVD equipment, and the lower part of the central air homogenizing column is fixedly connected through a central through hole of the lower disc; the central air homogenizing column is provided with a plurality of air holes communicated with each cabin, and the upper part of the central air homogenizing column is fixedly connected with the central air holes of the upper tray; the isolation sealing column is coaxially arranged with the central air homogenizing column and is used for sealing and isolating the upper disc and the lower disc.
In an embodiment of the present utility model, the function expanding part further includes a plurality of intermediate trays disposed in parallel between the upper tray and the lower tray, each of the intermediate trays having a hollow compartment structure, and having an upper side for loading the growth substrate and a lower side having a plurality of air outlet holes for air outflow;
each middle disc is fixed on the central air homogenizing column through a respective central through hole and is mutually communicated; the isolation sealing column is used for sealing and isolating the upper disc, the lower disc and the plurality of middle discs.
In the embodiment of the utility model, the upper disc, the lower disc and the plurality of middle discs are uniformly separated by the isolating seal column, and the vertical distance between the discs is 30-70mm.
In an embodiment of the present utility model, the vertical distance between the discs separated by the separation sealing column is 35-50mm.
In the embodiment of the utility model, two ends of the isolation sealing column are respectively in interference fit with circles recessed by 1mm at the center of each disc.
In an embodiment of the utility model, the lower plate has a solid structure, and the upper side is provided with a sample groove for loading a growth substrate; the upper side of each middle disc is provided with a sample groove which is the same as that of the lower disc.
In the embodiment of the utility model, the sizes of the air outlet sieve holes of the upper disc and all the middle discs are 0.8-1.5mm, and the distances between the centers of the holes of two adjacent sieve holes are 3-5mm.
In the embodiment of the utility model, the sizes of the air outlet sieve holes of the upper disc and all the middle discs are 0.9-1.2mm, and the distances between the centers of the holes of two adjacent sieve holes are 3-4mm.
In the embodiment of the utility model, the upper disc and all the middle discs are respectively provided with 4 hollow separation cabins; the central air homogenizing column is provided with 4 air holes corresponding to the middle discs and the upper discs in a matching way, so that the air flow is evenly divided equally.
The utility model also provides a graphene film growth device, which comprises a sealed cavity, wherein an induction heating area is arranged in the cavity; the induction heating zone is provided with a function expanding part of the bubble CVD equipment;
the cavity is connected with an air inlet device, and the air inlet device is used for introducing the hydrocarbon mixed gas into the induction heating area; the cavity is also connected with a cooling device for cooling the gas mixture generated by the reaction.
Compared with the prior art, the function expansion component suitable for the BCVD equipment provided by the embodiment of the utility model consists of an upper disc, a lower disc, a plurality of middle discs, a central air homogenizing column, an isolation sealing column and other components, wherein one surfaces of the upper disc and each middle disc are provided with air outlet sieve holes, the inside of the upper disc is provided with a separation cavity structure, and the problems of uneven air mixing, uneven film growth caused by uneven flow and low quality are perfectly solved by combining the central air homogenizing column, the isolation sealing column and the like. By combining the characteristics of BCVD, the design and addition of the novel component of the embodiment of the utility model can solve the problem of single function of equipment and solve the problems of the traditional hot wall CVD and cold wall CVD. The component has reasonable design and modular assembly, and is an expansion component for preparing the metal and nonmetal-based graphene films in batches simply, efficiently and multifunctional. Through practice, the upper, middle and lower three disc surfaces of the function expansion part can provide 16 thin film growth positions in total, and the full utilization of axial space is realized in the effective space of the current design of the equipment.
Drawings
FIG. 1 is a schematic diagram of the overall topography profile of a design component provided by an embodiment of the present utility model;
FIG. 2 is a cross-sectional view A-A of FIG. 1;
FIG. 3 is a schematic view of the structure of the intermediate plate of the component according to the embodiment of the present utility model;
FIG. 4 is a cross-sectional view A-A of FIG. 3;
FIG. 5 is a section B-B of FIG. 4;
FIG. 6 is a scanning electron microscope image of a 4 inch copper-based graphene film grown by the component according to an embodiment of the present utility model;
FIG. 7 is a graph of a Raman characterization of a 4 inch copper-based graphene film grown by the component according to an embodiment of the present utility model.
Detailed Description
The following description of the embodiments of the present utility model will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
In the description of the present utility model, it should be understood that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientation or positional relationship based on that shown in the drawings, are merely for convenience of describing the present utility model and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present utility model.
The utility model provides a function expansion part of bubble CVD equipment, which is positioned in a cavity of the bubble CVD equipment and comprises an upper disc, a lower disc, a central gas homogenizing column and an isolation sealing column;
the upper disc is provided with a hollow separation cabin structure, the upper side of each cabin is close to the upper part of the cavity of the bubble CVD equipment, and the lower side of each cabin is provided with a plurality of air outlet sieve holes for air outflow; the lower disc is arranged in parallel corresponding to the lower side of the upper disc and is used for loading a growth substrate;
the upper end of the central air homogenizing column is communicated and fixed with a corresponding interface of the bubble CVD equipment, and the lower part of the central air homogenizing column is fixedly connected through a central through hole of the lower disc; the central air homogenizing column is provided with a plurality of air holes communicated with each cabin, and the upper part of the central air homogenizing column is fixedly connected with the central air holes of the upper tray; the isolation sealing column is coaxially arranged with the central air homogenizing column and is used for sealing and isolating the upper disc and the lower disc.
The utility model provides a BCVD function expanding component (namely a function expanding component of bubble CVD equipment), and provides a growth preparation device and a method of a 4-inch metal and nonmetal substrate graphene film by combining the characteristics of rapid temperature rise and reduction, large growth cavity, normal pressure growth and industrial production capacity of the BCVD equipment. The utility model not only can solve the problems of single functions and products of BCVD equipment, but also can solve the problems of small scale, experimental level, serious gas phase parasitic reaction and low film surface cleanliness of the traditional hot wall CVD equipment, and can also solve the problems of low temperature rise and low temperature drop, low gas supply rate and inapplicability to the normal pressure growth of an insulating substrate and long growth period of the traditional cold wall CVD equipment.
Referring to fig. 1 and fig. 2, fig. 1 is a schematic diagram of an overall profile of a design component according to an embodiment of the present utility model, which is located in a BCVD apparatus cavity (but the BCVD apparatus is not shown in the drawings); fig. 2 is a section A-A of fig. 1. Wherein, 1 is the upper disc, 2 is the lower disc, 3 is an intermediate disc, 4 is the central even gas column, 5 is the isolation seal column, and 6 is the fastener.
The function expansion part comprises structural parts such as an upper disc 1, a lower disc 2, a middle disc 3, a central gas homogenizing 4, an isolation sealing column 5 and the like; wherein, the upper disc 1 is a disc-shaped part close to the upper part or upper end of the cavity of the BCVD device, and is in a hollow separated cabin structure, a plurality of air outlet sieve holes, preferably a plurality of uniform distribution, are arranged at the lower side of each cabin, play roles in homogenizing gas and similar liquid spraying, and can provide 'spraying' for growth gas on the next adjacent layer. Specifically, the sizes of the air outlet sieve holes of the upper disc are all 0.8-1.5mm, preferably 1mm. And the radial and axial distances of the air outlet sieve holes are 3-5mm, preferably 3mm.
The disc-shaped part which is arranged in parallel corresponding to the lower side of the upper disc 1 is a lower disc 2 which is positioned below the inner part of the cavity of the BCVD equipment and mainly plays a role in loading the growth substrate. The lower tray according to the embodiment of the utility model is not provided with a hollow structure, i.e. has a solid structure, and preferably has one or more sample wells on the upper side for loading the growth substrate.
The function expansion part according to the embodiment of the utility model further comprises: a number of intermediate discs 3 arranged in parallel between the upper disc 1 and the lower disc 2, 3 layers or 3 parallel intermediate disc-like parts being shown in the figure; each of said intermediate trays 3 has both a gas homogenizing and "spraying" action and a sample tank acting as a loading growth substrate. I.e. the intermediate plate 3 has a hollow compartment structure with an upper side (upper surface) for loading the growth substrate, receiving the growth gas "sprayed" under the last disc-shaped part, and a lower side (lower surface) designed with several gas outlet holes (also called "spraying" holes) for the gas outflow. In embodiments of the present utility model, the upper, middle and lower trays differ only in structure and function they assume. The sizes of the air outlet sieve holes of the upper disc and all the middle discs are 0.8-1.5mm, further 0.9-1.2mm, and preferably 1mm; and the radial and axial distances are 3-5mm, and further 3-4mm. The sieve holes are generally circular air outlet holes, and the size of 0.8-1.5mm is the diameter of the air outlet sieve holes; and the radial and axial distances are the distances between the centers of two adjacent sieve holes.
And, the upper side of each middle plate is provided with the same sample grooves as the lower plate, preferably 4 sample grooves with uniform size, and the thickness of the sample grooves is set according to the thickness of the film. 3-5, FIG. 3 is a schematic view of the structure of the intermediate plate of the component according to the embodiment of the present utility model; FIG. 4 is a cross-sectional view A-A of FIG. 3; fig. 5 is a sectional view of B-B of fig. 4.
The embodiment of the utility model is communicated and fixed with a corresponding interface of BCVD equipment through the upper end of the central gas homogenizing column 4; the lower part of the central air homogenizing column 4 is fixedly connected through a central through hole of the lower disc 2; the central air homogenizing column 4 is in a hollow column shape or a rod shape, is provided with a plurality of air holes communicated with each cabin, and the upper part of the central air homogenizing column is fixedly connected through a central through hole of the upper disc 1. Each of the intermediate disks 3 is fixed to the central gas-homogenizing column 4 through a respective central through hole and communicates with each other.
In the embodiment of the utility model, the upper disc 1 and all the middle discs 3 are respectively provided with 4 hollow separation cabins; the central air homogenizing column 4 is provided with 4 air holes corresponding to the middle discs and the upper discs in a matching way, so that the air flow is evenly and evenly divided into 4 hollow cabin cavities. Of course, other numbers of compartments may be provided in embodiments of the present utility model, such as 2, 3, 5, 6, etc.
Meanwhile, an isolation sealing column 5 is coaxially arranged with the central air homogenizing column 4 and is used for sealing and isolating the upper disc 1, the lower disc 2 and the plurality of middle discs 3. In the embodiment of the present utility model, the isolation seal 5 mainly serves to space the disks apart by a suitable distance, and the vertical distance between the disks is preferably 30-70mm, more preferably 35-50mm, and most preferably 40mm. Too close a distance can easily cause the sprayed growth gas to excessively contact with the growth substrate under pyrolysis, which can cause uneven thickness of the sample undulating region and macroscopic amorphous carbon attached islands on the substrate surface; too far does not provide good film forming ability because the growth rate of the graphene film under normal pressure growth is mainly determined by the nucleation rate of graphene on the substrate surface, and the migration and diffusion ability of molecules under normal pressure is insufficient and the free path is low.
It should be noted that the distance between the discs described herein may be calculated from the middle of the discs, the thickness of the upper disc and the middle disc being generally 5-10mm, preferably 8mm, the lower disc only taking charge and the thickness may be 3-5mm, preferably 4mm.
In addition, the two ends of the isolation sealing column 5 are respectively in interference fit with the circles which are concave by 1mm and are arranged at the centers of the discs, so that the sealing effect is achieved. The above-mentioned parts according to the embodiments of the present utility model are manufactured by using conventional materials suitable for CVD and BCVD, and the sizes of the parts are not particularly limited. In the central homogenizing column, 1000-6000sccm Ar or N can be introduced 2 50-300sccm methane and 10-100sccm hydrogen, and sealing by an isolation sealing column, wherein all parts can be assembled and matched into a whole.
The embodiment of the utility model adopts a modularized design, and is easy to install, disassemble and maintain. For example, the installation may be performed in a sequential order from bottom to top, that is, the lower fixing nut is assembled with the central gas homogenizing column 4, then the lower disc 2 is put in from the upper end, then the isolation seal column 5 is put in, then the middle disc 3, the isolation seal column 5, the middle disc 3, the upper disc 1, and the upper fastening nut 6 are put in. During installation, fine adjustment is needed to ensure that each of the sub-capsule cavities of the upper disc and the middle disc is aligned with the air holes of the central air homogenizing column in the vertical and horizontal directions, and the air outlet sieve pore areas are aligned with the sample grooves. The function expansion component is simple in structure, reasonable in design, high in utilization rate of axial space of the cavity, and capable of producing 16 four-inch graphene films at a time.
The embodiment of the utility model also provides a graphene film growth device, which comprises a sealed cavity, wherein an induction heating area is arranged in the cavity; the induction heating zone is provided with a function expanding part of the bubble CVD equipment; the cavity is connected with an air inlet device, and the air inlet device is used for introducing the hydrocarbon mixed gas into the induction heating area; the cavity is also connected with a cooling device for cooling the gas mixture generated by the reaction.
The crucible mentioned in the previous patent CN202110832518.1 is just a container, and the heating area is an induction heating coil, its graphite material can be heated in electromagnetic induction heating, in addition, copper blocks in the crucible can also be heated by induction heating, the crucible mainly provides the function of holding the copper blocks after melting into copper liquid, so that the late aerator device stretches into the copper liquid to foam, and graphene powder is produced. A crucible can be placed in an induction heating coil to produce graphene powder by a BCVD method, and the components disclosed by the embodiment of the utility model can be placed to prepare a graphene film by an atmospheric pressure method, so that the growth and preparation of 16-piece 4-inch metal-based/nonmetal-based graphene films can be realized.
Wherein, the crucible in the prior patent CN202110832518.1 is replaced by the function expanding component; the component is made of graphite, and can be placed in the middle of the induction coil to realize temperature-controllable heating, so that the nonmetallic substrate is indirectly heated. For the connection of the component, the connection can be carried out with the corresponding interface of the BCVD main body equipment through M24 x 1.5 threads at the upper end of the central gas homogenizing column.
And the specific contents of the air inlet device, the cooling device and the like are as described in the previous patent. For example, the cavity is connected with a vacuumizing device, and is provided with an observation window and the like. The air inlet device is connected with a barometer and comprises an air inlet pipe, an aerator and the like. The cooling device comprises a water cooling device, the water cooling device comprises a water cooling source, a circulating pipe and a water pump, the circulating pipe comprises a water cooling section wound at the upper end of the cavity, and the water cooling section is used for cooling a gas mixture, a film product and the like.
According to the embodiment of the utility model, the graphene film growth device is used for film preparation, and annealing and impurity removal treatment is needed after the first installation of the component, so that the graphene film growth device can be used for film preparation; the annealing impurity removal method comprises the following specific steps: placing the assembled parts into an induction heating zone of BCVD equipment, setting the heating temperature to 300 ℃, and introducing 1000sccm Ar or N during the heating 2 Keeping the temperature for 15 minutes after reaching 300 ℃, then setting the temperature to 600 ℃, keeping the temperature for 15 minutes, setting the temperature to 1400 ℃ immediately, keeping the temperature for 60 minutes, cooling to room temperature after finishing, and taking out.
In the embodiment of the utility model, the graphene film growth device is used for film growth, and the technological step parameters such as gas flow, proportion, growth process and the like in preparation can be regulated and controlled according to requirements. Wherein the metal substrate comprises copper, gold, nickel, cobalt, molybdenum, titanium, platinum and other metals with catalytic capability, carbon dissolving capability or interfacial interaction and alloys thereof; the nonmetallic substrate includes sapphire, silicon/silicon dioxide, glass, titanium dioxide, etc.
The metal substrate growth according to some embodiments of the present utility model comprises the following specific steps of: cutting 16 pieces of copper foil with a thickness of 25-500 μm and a size of 4 inches, placing in a sample tank designed by the component, and vacuumizing to 10 -3 Pa back pass 80000sccmAr or N 2 Restoring normal pressure, and then adjusting Ar or N 2 The flow is 1000-10000sccm, induction heating is started to raise the temperature to 980-1060 ℃, the temperature is kept for 45 minutes, and Ar or N of 1000-6000sccm is introduced after the temperature is kept 2 And (3) 50-300sccm of methane and 10-100sccm of hydrogen, after 5-30 minutes of growth, closing the hydrogen and methane, closing induction heating, cooling water in a circulating way, cooling to room temperature, and taking out.
According to other embodiments of the present utility model, a specific step of growing a non-metal substrate with sapphire comprises: 16 pieces of Al with the thickness of 0.5-1.5 and the size of 4 inches are clamped 2 O 3 Placing the substrate in a sample tank designed by the component, vacuumizing to 10 -3 Pa back pass 80000sccmAr or N 2 Restoring normal pressure, and then adjusting Ar or N 2 The flow is 2000-8000sccm, the induction heating is started to raise the temperature to 1100-1400 ℃, the temperature is kept for 45 minutes, and Ar or N is added after the temperature is kept 2 The flow rate of (2) is adjusted to 2000-8000sccm, and 10-80sccm H is introduced 2 And additionally 200-1000sccm Ar or N 2 Introducing into a bubbling device, loading ethanol vapor into a growth cavity, growing for 30-120 min, closing hydrogen and ethanol, closing induction heating, cooling with cooling water, cooling with circulating water, and taking out to room temperature.
The function expansion component is combined with the characteristics of the BCVD equipment, and can be used for preparing metal and nonmetal-based high-quality graphene films. The design of the component innovatively expands the functions of the bubble CVD equipment, so that the function of the bubble CVD equipment is diversified, and besides the original preparation of powder, the production and the preparation of 16 graphene films with the size of 4 inches can be provided at a time in the current effective growth space.
In order to better understand the technical content of the present utility model, the following provides specific examples to further illustrate the present utility model. In the following examples, all the raw materials used are commercially available.
The function expansion part of the bubble CVD equipment provided by the embodiment of the utility model is integrally composed of an upper disc, a three-layer middle disc, a lower disc, a central gas homogenizing column, a fastener and an isolation sealing column, and adopts graphite materials and a modularized design. Wherein the vertical distance between the discs isolated by the isolating sealing column is 40mm; and two ends of the isolation sealing column are respectively in interference fit with circles which are concave by 1mm and are arranged at the centers of the discs. The sizes of the air outlet sieve holes of the upper disc and all the middle discs are 1mm, and the radial and axial distances are 3mm; the upper disc and all the middle discs are respectively provided with 4 hollow separation cabins; the central air homogenizing column is provided with 4 air holes corresponding to the positions of the middle discs and the upper discs in a matching way. The lower disc is of a solid structure, and a sample groove for loading a growth substrate is formed in the upper side of the lower disc; the upper side of each middle disc is provided with a sample groove which is the same as that of the lower disc.
Example 1
Cutting 16 pieces of copper foil with the thickness of 50um and the size of 4 inches, placing the copper foil in a sample groove designed by the component, and vacuumizing to 10 -3 Pa back pass 80000sccmN 2 Restoring normal pressure, and then adjusting N 2 The flow is 2000sccm, the induction heating is started to raise the temperature to 1040 ℃, the temperature is kept for 45 minutes, and after the temperature is kept, the temperature is kept at 2000sccm N originally 2 On the basis of the above, 100sccm of methane and 50sccm of hydrogen are introduced, after 5 minutes of growth, the hydrogen and methane are closed, induction heating is closed, cooling water is circulated, water is cooled to room temperature, and the mixture is taken out. SEM characterization and Raman characterization were performed on the films after growth, and the results are shown in fig. 6 and 7. From fig. 6, it can be seen that the typical wrinkle morphology of the copper-based graphene film, in which white small bright spots are the result of condensing copper vapor on the film surface during the cooling process at high temperature, can be removed later by dilute hydrochloric acid washing. Advancing oneFurther, from the Raman spectral characterization of fig. 7, it can be seen that the typical Raman characteristic peak of graphene, the film was not transferred to Si/SiO 2 Raman characterization was performed and the peak was not back-ground.
Example 2
16 pieces of Al with the thickness of 0.5mm and the size of 4 inches are clamped 2 O 3 Placing the substrate in a sample tank designed by the component, vacuumizing to 10 -3 After Pa, the flow rate of Ar is adjusted to 2000sccm, induction heating is started to raise the temperature to 1300 ℃, the temperature is kept for 45 minutes, after the heat preservation is finished, the flow rate of Ar is adjusted to 4000sccm, and H of 85sccm is introduced 2 And in addition, 500sccm Ar is introduced into a bubbling device to load ethanol vapor into a growth cavity, hydrogen and ethanol are closed after the growth is carried out for 45 minutes, induction heating is closed, cooling water is cooled to room temperature in a circulating way, and the ethanol vapor is taken out.
According to the embodiment, the upper, middle and lower three disc surfaces of the function expansion component can provide 16 thin film growth positions in total, the growth preparation method of the 4-inch metal and nonmetal base graphene thin film is provided, 16 4-inch graphene thin films can be produced and prepared at one time, and the full utilization of the axial space is realized in the effective space of the current design of equipment. By combining the characteristics of BCVD, the design and addition of the novel component of the embodiment of the utility model can solve the problem of single function of equipment and solve the problems of the traditional hot wall CVD and cold wall CVD. The component has reasonable design and modular assembly, and is an expansion component for preparing the metal and nonmetal-based graphene films in batches simply, efficiently and multifunctional.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present utility model. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the utility model. Thus, the present utility model is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The function expanding component of the bubble CVD equipment is positioned in the cavity of the bubble CVD equipment and is characterized by comprising an upper disc, a lower disc, a central air homogenizing column and an isolation sealing column;
the upper disc is provided with a hollow separation cabin structure, the upper side of each cabin is close to the upper part of the cavity of the bubble CVD equipment, and the lower side of each cabin is provided with a plurality of air outlet sieve holes for air outflow; the lower disc is arranged in parallel corresponding to the lower side of the upper disc and is used for loading a growth substrate;
the upper end of the central air homogenizing column is communicated and fixed with a corresponding interface of the bubble CVD equipment, and the lower part of the central air homogenizing column is fixedly connected through a central through hole of the lower disc; the central air homogenizing column is provided with a plurality of air holes communicated with each cabin, and the upper part of the central air homogenizing column is fixedly connected with the central air holes of the upper tray; the isolation sealing column is coaxially arranged with the central air homogenizing column and is used for sealing and isolating the upper disc and the lower disc.
2. The function expanding member according to claim 1, further comprising a plurality of intermediate trays arranged in parallel between the upper tray and the lower tray, each of the intermediate trays having a hollow compartment structure, and an upper side for loading the growth substrate and a lower side having a plurality of gas outlet holes for gas outflow;
each middle disc is fixed on the central air homogenizing column through a respective central through hole and is mutually communicated; the isolation sealing column is used for sealing and isolating the upper disc, the lower disc and the plurality of middle discs.
3. The function expanding unit of claim 2, wherein the isolating seal column uniformly separates the upper plate, the lower plate and the plurality of intermediate plates, and a vertical distance between the plates is 30-70mm.
4. A function expanding unit according to claim 3, wherein the vertical distance between the discs separated by the separation sealing column is 35-50mm.
5. A function expanding member according to claim 3, wherein both ends of the isolation seal column are respectively interference fitted with a circle recessed by 1mm at the center of each disc.
6. The function expanding member according to any one of claims 2 to 5, wherein the lower plate has a solid structure and is provided with a sample tank for loading a growth substrate at an upper side; the upper side of each middle disc is provided with a sample groove which is the same as that of the lower disc.
7. The function expanding member according to any one of claims 2 to 5, wherein the vent screening holes of the upper tray and all intermediate trays are each 0.8 to 1.5mm in size, and the distance between the centers of the holes of adjacent two screening holes is 3 to 5mm.
8. The function expanding member according to claim 7, wherein the vent holes of the upper tray and all the intermediate trays are each 0.9-1.2mm in size and the distance between the hole centers of the adjacent two sieve holes is 3-4mm.
9. The function expanding member according to any one of claims 2-5, wherein the upper disc and all intermediate discs are each provided with 4 hollow compartments; the central air homogenizing column is provided with 4 air holes corresponding to the middle discs and the upper discs in a matching way, so that the air flow is evenly divided equally.
10. The graphene film growth device is characterized by comprising a sealed cavity, wherein an induction heating area is arranged in the cavity; the induction heating zone is provided with a function expanding part of the bubble CVD apparatus according to any one of claims 1 to 9;
the cavity is connected with an air inlet device, and the air inlet device is used for introducing the hydrocarbon mixed gas into the induction heating area; the cavity is also connected with a cooling device for cooling the gas mixture generated by the reaction.
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