Graphene film casing deposition device and preparation method
Through the sleeve-type plasma enhanced chemical vapor deposition device, the radio frequency coil is clamped between the inner and outer sleeves, which solves the problems of low preparation efficiency and safety hazards in PECVD and realizes efficient and safe graphene film preparation.
Patent Information
- Application Number
- CN202210135346.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-02-14
- Publication Date
- 2025-09-16
- Estimated Expiration
- 2042-02-14
AI Technical Summary
In existing PECVD devices for preparing graphene films, the separation of the plasma excitation coil and the heating zone results in low preparation efficiency, and there are safety hazards such as the radio frequency coil being deformed by heat or coming into contact with the metal substrate.
A sleeve-type plasma enhanced chemical vapor deposition device is used, and a radio frequency coil is clamped between inner and outer sleeves to achieve overlap of the plasma space and the high-temperature environment. At the same time, the radio frequency coil is isolated from the metal substrate and the heating furnace resistance wire to avoid safety accidents.
The preparation efficiency of graphene films is improved, the service life of radio frequency coils is extended, production safety is ensured, and costs are reduced.
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Figure CN116621165B_ABST
Abstract
Description
Technical Field
[0001] The present application relates to a graphene film preparation device and preparation method, and specifically, to a sleeve-type plasma enhanced chemical vapor deposition device and preparation method for graphene films. Background Art
[0002] Graphene, a single-atom-thick layer of graphite with a hexagonal honeycomb lattice, possesses exceptional physical and chemical properties due to its unique microstructure. Graphene exhibits excellent thermal and chemical stability, and exhibits low shear forces between layers. Therefore, graphene holds great potential in corrosion resistance and friction reduction. Graphene's exceptional properties and promising applications have sparked significant interest in the preparation of high-quality, large-area, long-range ordered graphene films.
[0003] Plasma-enhanced chemical vapor deposition (PECVD) is a method for producing graphene using radiofrequency plasma-assisted chemical vapor deposition. This method utilizes plasma to effectively cleave precursor molecules, lowering the chemical reaction barrier and enabling film formation at relatively low temperatures. Common plasma sources include microwave, radiofrequency, and direct current discharge (DC). These are referred to as WPCVD, RF-PECVD, and DC-PECVD, depending on the plasma source. RF-PECVD reduces the cost of producing graphene films by achieving low-temperature growth and offers advantages such as high film quality, large growth area, and high transparency. It also significantly increases the potential for large-scale production of high-quality graphene on substrates that are not heat-resistant, facilitating the industrial production and practical applications of graphene. Specifically, methane and hydrogen are introduced. Under the influence of an RF electric field, the hydrogen is ionized into ions, enhancing plasma activity and accelerating the reaction. The electrons accelerated by the RF field have kinetic energies exceeding 10 eV, breaking the carbon-hydrogen bonds of most methane molecules, depositing carbon atoms on the substrate to form graphene films.
[0004] In PECVD systems for graphene film deposition, the separation of the plasma excitation coil from the heating zone results in low film deposition efficiency. Placing the RF coil within the heating zone requires design support and can easily cause the coil to deform due to heat, potentially contacting the metal substrate or the heating resistor wire of the heating furnace, leading to safety hazards. Therefore, there is an urgent need for a plasma-enhanced chemical vapor deposition (PECVD) system for graphene film deposition that can both place the plasma excitation coil within the heating furnace and isolate the RF coil from the metal substrate and the heating resistor wire. Summary of the Invention
[0005] A main purpose of the present application is to overcome at least one of the defects of the above-mentioned prior art and to provide a sleeve-type plasma enhanced chemical vapor deposition device that can both improve the efficiency of graphene film preparation and avoid safety accidents.
[0006] To achieve the above objectives, this application adopts the following technical solutions:
[0007] According to one aspect of the present application, a sleeve-type plasma-enhanced chemical vapor deposition apparatus for preparing graphene films is provided, comprising an unwinding chamber, a rewinding chamber, an inner sleeve, an outer sleeve, and a radio frequency coil. The unwinding chamber is provided with an unwinding wheel, the rewinding chamber is provided with a rewinding wheel, the inner sleeve sealably connects the unwinding chamber and the rewinding chamber, the outer sleeve is provided externally of the inner sleeve, and the radio frequency coil is helically disposed between the inner sleeve and the outer sleeve.
[0008] According to one embodiment of the present application, the inner sleeve and the outer sleeve are both made of high-temperature resistant rigid material.
[0009] According to one embodiment of the present application, the inner diameter of the outer sleeve is D, the outer diameter of the inner sleeve is d, and the diameter of the winding of the RF coil is t, wherein D>d+2t.
[0010] According to one embodiment of the present application, the inner diameter of the outer sleeve is 9.5 cm-11 cm, and the inner diameter of the inner sleeve is 6.5 cm-8 cm.
[0011] According to one embodiment of the present application, a protrusion for fixing the winding position of the radio frequency coil is provided on the inner wall of the outer sleeve.
[0012] According to one embodiment of the present application, the sleeve-type plasma enhanced chemical vapor deposition apparatus further includes a heating furnace disposed between the unwinding bin and the winding bin, the heating furnace accommodating the outer sleeve and the RF coil, and the inner sleeve passing through the heating furnace.
[0013] According to an embodiment of the present application, the length of the RF coil is shorter than the length of the heating chamber of the heating furnace, and the distance between the end of the RF coil and the inner wall of the heating chamber corresponding to the end is 8-12 cm.
[0014] According to an embodiment of the present application, a distance between an end of the RF coil and an inner wall of the heating chamber corresponding to the end is 10 cm.
[0015] According to one embodiment of the present application, pipe plugs are provided at both ends of the inner sleeve, and a slit for allowing the substrate to pass through is provided in the middle of the pipe plug.
[0016] According to another aspect of the present application, a method for preparing a graphene film is provided, using the aforementioned telescoped plasma enhanced chemical vapor deposition apparatus, and the specific steps are as follows:
[0017] Step 1: placing the substrate on the unwinding wheel in the unwinding bin;
[0018] Step 2: Pass the substrate through the inner sleeve and connect it to the winding wheel in the winding bin;
[0019] Step 3: Introduce protective gas, start heating and introduce carbon source atmosphere. When the temperature inside the inner tube reaches the preparation temperature, turn on the RF coil;
[0020] Step 4: preparing a graphene film. During the preparation process, the winding wheel winds up the substrate and the graphene film deposited on the substrate.
[0021] As can be seen from the above technical solutions, the advantages and positive effects of the telescopic plasma-enhanced chemical vapor deposition device and preparation method of graphene film proposed in this application are:
[0022] The present invention proposes a sleeve-type plasma-enhanced chemical vapor deposition apparatus for graphene film, comprising an unwinding chamber, a rewinding chamber, an inner sleeve, an outer sleeve, and a radio frequency coil. The unwinding chamber is provided with an unwinding wheel for mounting a substrate; the rewinding chamber is provided with a rewinding wheel for rewinding the substrate with the graphene film attached thereto. The inner sleeve seals and connects the unwinding chamber and the rewinding chamber to ensure a suitable environment for preparing the graphene film. The outer sleeve is provided outside the inner sleeve, and the radio frequency coil is spirally arranged between the inner sleeve and the outer sleeve. By spirally arranging the radio frequency coil between the inner sleeve and the outer sleeve, the radio frequency coil, the inner sleeve, and the outer sleeve are all arranged within the heating region during the preparation of the graphene film. This allows the plasma space and the high-temperature environment to overlap while effectively isolating and protecting the radio frequency coil. This improves the utilization efficiency of the plasma while extending the service life of the radio frequency coil, isolates the radio frequency coil from the substrate, and isolates the radio frequency coil from the heating equipment. This effectively improves the quality of the graphene film while extending the service life of the radio frequency coil and ensuring production safety. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] The above and other features and advantages of the present application will become more apparent by describing in detail example embodiments thereof with reference to the accompanying drawings.
[0024] Figure 1 It is a structural schematic diagram of the sleeve-type plasma enhanced chemical vapor deposition device of the present application.
[0025] Figure 2 yes Figure 1 Schematic diagram of the cross-sectional structure at AA in FIG.
[0026] The description of the accompanying drawings is as follows:
[0027] 100-tube plasma enhanced chemical vapor deposition device;
[0028] 101- unwinding warehouse;
[0029] 102- unwinding wheel;
[0030] 103-winding warehouse;
[0031] 104-rewinding wheel;
[0032] 105-inner casing;
[0033] 106- outer sleeve;
[0034] 107-RF coil;
[0035] 108-heating furnace;
[0036] 109-substrate;
[0037] 110-intake pipe;
[0038] 111-exhaust pipe;
[0039] 112-pipe blockage;
[0040] d-outer diameter of inner casing;
[0041] D-inner diameter of outer sleeve;
[0042] t - diameter of the wire of the RF coil. DETAILED DESCRIPTION
[0043] Typical embodiments that embody the features and advantages of the present application will be described in detail in the following description. It should be understood that the present application can have various variations in different embodiments without departing from the scope of the present application, and the description and drawings therein are essentially for illustrative purposes and not for limiting the present application.
[0044] In the following description of different exemplary embodiments of the present application, reference is made to the accompanying drawings, which form a part of the present application and in which different exemplary structures, systems and steps that can implement various aspects of the present application are shown by way of example. It should be understood that other specific schemes of components, structures, exemplary devices, systems and steps can be used, and structural and functional modifications can be made without departing from the scope of the present application. Moreover, although the terms "upper", "middle", "inner", etc. may be used in this specification to describe different exemplary features and elements of the present application, these terms are used herein for convenience only, for example, according to the direction of the examples described in the accompanying drawings. Nothing in this specification should be construed as requiring a specific three-dimensional orientation of the structure to fall within the scope of the present application.
[0045] In order to make the above-mentioned objects, features and advantages of the present application clear and easy to understand, the specific embodiments of the present application are described in detail below with reference to the accompanying drawings.
[0046] like Figure 1 As shown, the sleeve-type plasma-enhanced chemical vapor deposition apparatus 100 of the present application includes an unwinding chamber 101, a rewinding chamber 103, an inner sleeve 105, an outer sleeve 106, and a radio frequency coil 107. The unwinding chamber 101 is provided with an unwinding wheel 102 for mounting a substrate 109; the rewinding chamber 103 is provided with a rewinding wheel 104 for rewinding the substrate 109 with a graphene film attached thereto; the inner sleeve 105 seals and connects the unwinding chamber 101 and the rewinding chamber 103 to ensure a suitable environment for preparing the graphene film; the outer sleeve 106 is provided outside the inner sleeve 105 and does not require sealing; and the radio frequency coil 107 is provided in the space formed by the inner sleeve 105 and the outer sleeve 106. The use of a spiral arrangement of the radio frequency coil between the inner sleeve and the outer sleeve enables the overlap of the plasma space and the high-temperature environment space while effectively isolating and protecting the radio frequency coil, thereby improving the utilization efficiency of the plasma and extending the service life of the radio frequency coil. This effectively solves the problem of supporting the RF coil and prevents short circuits caused by contact between the substrate and the RF coil, thereby improving the safety of the device. In this embodiment, the substrate 109 is a metal foil, typically copper foil. In other embodiments, it can also be a lightweight metal such as aluminum foil, or nickel foil.
[0047] In this embodiment, the sleeve-type plasma-enhanced chemical vapor deposition apparatus 100 further includes a heating furnace 108, which is positioned between the unwinding chamber 101 and the rewinding chamber 103. An outer sleeve 106 and a radio frequency coil 107 are located within the heating furnace 108. The outer sleeve 106 protects the radio frequency coil 107 and prevents contact between the radio frequency coil 107 and the heating resistor wire of the heating furnace 108. An inner sleeve 105 extends through the heating furnace 108, sealingly connecting the unwinding chamber 101 and the rewinding chamber 103. This effectively isolates the graphene film substrate 109 from the radio frequency coil 107. The substrate 109 is positioned within the inner sleeve 105, extending from the unwinding chamber 101 to the rewinding chamber 103 along the axis of the inner sleeve 105. Accommodating the radio frequency coil in the heating furnace allows the plasma generation region and the high-temperature heating region to overlap and couple into a single zone, while effectively protecting the radio frequency coil. This improves plasma utilization efficiency and effectively protects the radio frequency coil, thereby extending the service life of the radio frequency coil. It can also isolate the RF coil from the metal substrate and the resistance wire of the heating furnace to avoid production accidents.
[0048] In this embodiment, the telescopic plasma-enhanced chemical vapor deposition apparatus 100 further includes an air inlet pipe 110 and an air extraction pipe 111. The air inlet pipe 110 is connected to the unwinding chamber 101 and to an external air source. The air extraction pipe 111 is connected to the winding chamber 103 and to an external air extraction device, which may be a vacuum pump, an air extractor, or the like.
[0049] In this embodiment, cooling water flanges (not shown in the figure) are provided at both ends of the heating furnace 108, and cylindrical pipe plugs 112 are provided at the connection between the inner sleeve 105 and the unwinding bin 101 and at the connection between the inner sleeve 105 and the winding bin 103. A slit is provided in the middle of the pipe plug 112 for the substrate 109 to pass through. The diameter of the pipe plug 112 is slightly smaller than the diameter of the inner sleeve 105, so as to achieve interlayer protection of the upper and lower cover plates for the substrate, ensure that the plasma is concentrated in the heating area, prevent the plasma from overflowing to the non-heating area, and reduce the contamination of the substrate by the low-temperature polymer.
[0050] In this embodiment, the end of the outer sleeve 106 needs to be thermally insulated and sealed to reduce heat loss. Quartz wool filling or quartz welding sealing can be used to reduce heat dissipation and ensure the stability of the heating environment temperature.
[0051] In this embodiment, a winding correction device (not shown) can be provided in the winding bin 103 to ensure smooth winding. A horizontal support frame (not shown) can also be provided below the substrate 109 in the heating area to support the substrate 109 and ensure that it is centered in the inner sleeve 105.
[0052] In this embodiment, the unwinding end of the unwinding bin and the winding end of the winding bin are both covered with grounded copper foil (not shown in the figure) to reduce the overflow of plasma. When the unwinding end is insulated, it is found that some plasma overflows along the substrate 109, resulting in certain low-temperature polymer contamination on the surface of the product. When both ends are fully grounded, the overflow of plasma in the unwinding bin is greatly reduced.
[0053] In this embodiment, both the inner sleeve 105 and the outer sleeve 106 are made of a high-temperature resistant rigid material, such as quartz, graphite, ceramic, or a high-temperature resistant alloy. Because the inner sleeve 105 and the outer sleeve 106 need to be heated during the graphene film preparation process, using a high-temperature resistant rigid material prevents the inner sleeve 105 and the outer sleeve 106 from deforming during high-temperature heating and thus failing to provide effective isolation and support.
[0054] In this embodiment, the RF coil 107 can be made of copper wire or silver-plated copper wire, and the plasma intensity can be increased by increasing the number of coils. The length of the RF coil 107 is shorter than the length of the heating chamber of the heating furnace 108, and the distance between the end of the RF coil 107 and the inner wall of the heating chamber corresponding to the end is 8-12 cm, preferably 10 cm, to prevent the plasma excited by the RF coil from overflowing to the ends of the heating zone and contaminating the substrate surface.
[0055] like Figure 2 As shown, the inner diameter of the outer sleeve 106 of the sleeve-type plasma-enhanced chemical vapor deposition apparatus 100 of the present application is D, the outer diameter of the inner sleeve 105 is d, and the diameter of the winding of the radio frequency coil 107 is t, where D>d+2t is required to be satisfied. This allows the radio frequency coil 107 to be arranged in the space formed by the inner sleeve 105 and the outer sleeve 106, and the diameter of the inner sleeve 105 and the diameter of the outer sleeve 106 cannot differ too much. In other words, the cylindrical space between the inner and outer sleeves only needs to be large enough to accommodate the radio frequency coil 107. Otherwise, a large amount of heat loss will be generated, which is not conducive to energy conservation and causes waste.
[0056] In this embodiment, the width of substrate 109 is smaller than the inner diameter of inner sleeve 105. Therefore, the inner diameter of the inner sleeve cannot be too small. Furthermore, since the diameters of inner sleeve 105 and outer sleeve 106 cannot differ significantly, the inner diameter of inner sleeve 105 can be made as large as possible. This allows the plasma excitation coil to be placed within the heating furnace, while isolating the RF coil from the metal substrate and the heating furnace resistance wire, and preventing the RF coil from affecting the width of the graphene film.
[0057] In this embodiment, the inner diameter of the inner sleeve 105 is 6.5 cm to 8 cm, preferably 7.5 cm, and the inner diameter of the outer sleeve is 9.5 cm to 11 cm, preferably 10 cm. The above data selections affect each other and, when used in combination, can achieve a wider width of the produced graphene film.
[0058] In this embodiment, a protrusion (not shown) is provided on the inner wall of the outer sleeve 106 to fix the position of the RF coil 107. This is used to reduce deformation of the RF coil due to high temperature during heating, avoid contact between coils, and maintain stable plasma intensity during the preparation process.
[0059] It should be noted that the sleeve-type plasma-enhanced chemical vapor deposition apparatuses shown in the drawings and described in this specification are merely a few examples of the many types of sleeve-type plasma-enhanced chemical vapor deposition apparatuses that can employ the principles of the present application. It should be clearly understood that the principles of the present application are in no way limited to any details of the sleeve-type plasma-enhanced chemical vapor deposition apparatuses shown in the drawings or described in this specification, or to any components of the sleeve-type plasma-enhanced chemical vapor deposition apparatuses.
[0060] The above is a detailed description of several exemplary embodiments of the sleeve-type plasma-enhanced chemical vapor deposition apparatus proposed in this application. The following is an exemplary description of the method for preparing the graphene film proposed in this application.
[0061] Combined with attachment Figures 1 to 2 The method for preparing the graphene film proposed in this application uses the above-mentioned telescoped plasma enhanced chemical vapor deposition device, and the specific steps are as follows:
[0062] Step 1: Place the substrate 109 on the unwinding wheel 102 in the unwinding chamber 101;
[0063] Step 2: Pass the substrate 109 through the inner sleeve 105 and connect it to the winding wheel 104 in the winding chamber 103;
[0064] Step 3: introduce protective gas, start heating and introduce carbon source atmosphere, and when the temperature inside the inner sleeve 105 reaches the preparation temperature, turn on the RF coil 107;
[0065] Step 4: preparing a graphene film. During the preparation process, the winding wheel 106 winds up the substrate 109 and the graphene film deposited on the substrate 109 .
[0066] In this embodiment, the preparation of the graphene film in step 4 can be prepared according to conventional steps in the prior art, or can be prepared by other steps, as long as the graphene film is prepared.
[0067] In this embodiment, the two ends of the RF coil 107 are connected to the transmitting end of the RF power supply and the ground end of the RF power supply respectively. After heating, the temperature inside the inner sleeve 105 needs to reach 600 degrees. The protective gas can be hydrogen or argon, and the carbon source atmosphere can be selected from methane, ethane, etc. The substrate 109 can be made of 8 to 10 transition metals (such as Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Au), and alloys (such as Co-Ni, Au-Ni, Ni-Mo, stainless steel). The main basis for selection is the melting point of the metal, the amount of carbon dissolved, and whether there is a stable metal carbide. These factors determine the growth temperature, growth mechanism and carrier gas type of graphene. In addition, the crystal type and crystal orientation of the metal will also affect the growth quality of graphene.
[0068] The following is a detailed description of the preparation reaction process using copper foil as the substrate and methane as the carbon source atmosphere:
[0069] CH4 molecules are adsorbed on the surface of the copper foil substrate, and the CH bonds break at high temperatures, producing various carbon fragments CHx; after the methane molecules are dehydrogenated, the carbon species on the copper foil surface aggregate with each other, generating new CC bonds and clusters, and begin to nucleate to form graphene islands; as the number of graphene nuclei on the copper foil surface increases, the carbon atoms or clusters produced subsequently continue to attach to the nucleation sites, causing the graphene nuclei to gradually grow until they suture each other. Suturing refers to the connection between the graphene nuclei as they gradually grow, forming larger graphene sheets, which are eventually connected into continuous graphene films.
[0070] Through the above-mentioned use process of the sleeve-type plasma enhanced chemical vapor deposition device of the present application and the preparation method of the graphene film, it can be concluded that the sleeve-type plasma enhanced chemical vapor deposition device of the present application is provided with inner and outer sleeves, and a radio frequency coil is clamped in the inner and outer sleeves. During the preparation process, the inner and outer sleeves with the radio frequency coil are placed in a heating furnace, achieving overlapping coupling of the heating area and the plasma excitation area while effectively isolating and protecting the radio frequency coil, improving the utilization rate of the plasma while extending the life of the radio frequency coil. The length of the heating area and the length of the plasma excitation area of the present application can be made equal, so that the heat in the heating area is fully utilized and the intensity of the plasma in the heating area is greatly improved.
[0071] In addition, the sleeve-type plasma enhanced chemical vapor deposition device of the present application can also reduce the low-temperature polymerized pollutants generated by the plasma overflowing into the heating zone and the two ends of the zone, so that the plasma generated by the excitation can fully participate in the generation of graphene film in the high-temperature heating zone. The sleeve-type plasma enhanced chemical vapor deposition device of the present application has a simple structural design, low processing precision requirements, a large material selectivity, flexible and convenient operation, and low cost. It can achieve the overlap of the RF excitation zone of the plasma with the high-temperature heating zone while protecting the RF coil and extending the life of the RF coil. It can also improve the utilization rate of the plasma while effectively isolating the RF coil from the metal substrate and the heating furnace resistance wire, avoiding production accidents and ensuring safe production.
[0072] In summary, the sleeve-type plasma-enhanced chemical vapor deposition device proposed in the present application includes an unwinding bin, a winding bin, an inner sleeve, an outer sleeve, and a radio frequency coil. An unwinding wheel is provided in the unwinding bin for installing a substrate; a winding wheel is provided in the winding bin for winding up a substrate with a graphene film attached thereto. The inner sleeve seals and connects the unwinding bin and the winding bin to ensure the preparation environment of the graphene film. The outer sleeve is provided on the outside of the inner sleeve, and the radio frequency coil is provided between the inner sleeve and the outer sleeve. During the preparation process, the inner and outer sleeves with the radio frequency coil sandwiched therebetween are arranged in a heating furnace, realizing overlapping coupling between the heating area and the plasma excitation area while effectively isolating and protecting the radio frequency coil, improving the utilization rate of the plasma while extending the life of the radio frequency coil. While improving the utilization rate of the plasma, the radio frequency coil is effectively isolated from the metal substrate and the resistance wire of the heating furnace, avoiding the occurrence of production accidents, improving production efficiency, and being conducive to saving energy and reducing costs.
[0073] The method for preparing a graphene film proposed in this application utilizes the aforementioned sleeve-type plasma-enhanced chemical vapor deposition apparatus, wherein a substrate is placed on an unwinding wheel in an unwinding chamber and connected to a rewinding wheel in a rewinding chamber through an inner sleeve; a protective gas is then introduced, heating is started, and a carbon source atmosphere is introduced. When the temperature in the inner sleeve reaches the preparation temperature, the radio frequency coil is turned on; the graphene film can then be prepared according to conventional steps. During the preparation process, the rewinding wheel rewinds the substrate and the graphene film deposited on the substrate. This method overlaps the radio frequency region with the heating region while protecting and effectively isolating the radio frequency coil. This method can efficiently utilize plasma and heat, save energy, and reduce costs. This method is beneficial for both improving the quality of the graphene film and ensuring production safety.
[0074] The exemplary embodiments of the sleeve-type plasma enhanced chemical vapor deposition apparatus and the method for preparing graphene films proposed in the present application are described and / or illustrated in detail above. However, the embodiments of the present application are not limited to the specific embodiments described herein. On the contrary, the components and / or steps of each embodiment can be used independently and separately from the other components and / or steps described herein. Each component and / or each step of an embodiment can also be used in combination with other components and / or steps of other embodiments. When introducing the elements / components / etc. described and / or illustrated herein, the terms "one", "first", "second" and "above" are used to indicate the presence of one or more elements / components / etc. The terms "comprising", "including" and "having" are used to indicate an open-ended inclusive meaning and mean that in addition to the listed elements / components / etc., additional elements / components / etc. may be present.
[0075] The embodiments of the present application are not limited to the specific embodiments described herein. On the contrary, the components of each embodiment can be used independently and separately from the other components described herein. Each component of an embodiment can also be used in combination with other components of other embodiments. In the description of this specification, the description of the terms "one embodiment", "some embodiments", "other embodiments" and the like means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the embodiment. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0076] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.
Claims
1. A telescoped plasma-enhanced chemical vapor deposition apparatus for preparing graphene films, characterized in that: include: An unwinding bin, wherein an unwinding wheel is provided in the unwinding bin; A winding bin, wherein a winding wheel is provided in the winding bin; An inner sleeve, the inner sleeve sealingly connecting the unwinding bin and the rewinding bin; an outer sleeve, disposed outside the inner sleeve; a radio frequency coil, the radio frequency coil being helically disposed between the inner sleeve and the outer sleeve; A heating furnace is provided between the unwinding bin and the winding bin, the heating furnace accommodates the outer sleeve and the radio frequency coil, and the inner sleeve passes through the heating furnace.
2. The telescoped plasma enhanced chemical vapor deposition apparatus according to claim 1, wherein: The inner sleeve and the outer sleeve are both made of high-temperature resistant rigid material.
3. The telescoped plasma enhanced chemical vapor deposition apparatus according to claim 1, wherein: The inner diameter of the outer sleeve is D, the outer diameter of the inner sleeve is d, and the diameter of the winding of the radio frequency coil is t, wherein D>d+2t.
4. The telescoped plasma enhanced chemical vapor deposition apparatus according to claim 1, wherein: The inner diameter of the outer sleeve is 9.5 cm-11 cm, and the inner diameter of the inner sleeve is 6.5 cm-8 cm.
5. The telescoped plasma enhanced chemical vapor deposition apparatus according to claim 1, wherein: A protrusion for fixing the winding position of the radio frequency coil is provided on the inner wall of the outer sleeve.
6. The telescoped plasma enhanced chemical vapor deposition apparatus according to claim 1, wherein: The length of the radio frequency coil is shorter than the length of the heating chamber of the heating furnace, and the distance between the end of the radio frequency coil and the inner wall of the heating chamber corresponding to the end is 8-12 cm.
7. The telescoped plasma enhanced chemical vapor deposition apparatus according to claim 6, wherein: The distance between the end of the RF coil and the inner wall of the heating chamber corresponding to the end is 10 cm.
8. The telescoped plasma enhanced chemical vapor deposition apparatus according to claim 1, wherein: Pipe plugs are provided at both ends of the inner sleeve, and a slit for allowing a substrate to pass through is provided in the middle of the pipe plug.
9. A method for preparing a graphene film, characterized in that: The telescopic plasma enhanced chemical vapor deposition apparatus according to any one of claims 1 to 8 is used, and the specific steps are as follows: Step 1: placing the substrate on the unwinding wheel in the unwinding bin; Step 2: Pass the substrate through the inner sleeve and connect it to the winding wheel in the winding bin; Step 3: Introduce protective gas, start the heating furnace and introduce carbon source atmosphere. When the temperature inside the inner sleeve reaches the preparation temperature, turn on the RF coil; Step 4: preparing a graphene film. During the preparation process, the winding wheel winds up the substrate and the graphene film deposited on the substrate.
Citation Information
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