CN111484003A - Dielectric barrier discharge graphene preparation device and preparation method - Google Patents
Dielectric barrier discharge graphene preparation device and preparation method Download PDFInfo
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- CN111484003A CN111484003A CN202010245255.XA CN202010245255A CN111484003A CN 111484003 A CN111484003 A CN 111484003A CN 202010245255 A CN202010245255 A CN 202010245255A CN 111484003 A CN111484003 A CN 111484003A
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Abstract
The invention provides a device and a method for preparing dielectric barrier discharge graphene, and belongs to the technical field of graphene preparation. The method solves the problems that the existing graphene preparation is difficult to be carried out under atmospheric pressure, and simultaneously has pollution and material defects. The device comprises a plasma processing chamber, a gas supply system, a power supply system and a detection and analysis system, wherein the plasma processing chamber adopts a structure of combining a horizontal flat capacitor with a dielectric barrier discharge, the plasma processing chamber comprises an upper electrode, a quartz medium, a mica sheet and a lower electrode, the upper electrode and the lower electrode are respectively connected with two ends of the power supply system, a discharge area is arranged between the upper electrode and the lower electrode, a palladium film is deposited on the surface of the quartz medium, the quartz medium is connected with the electrodes, a monomolecular carbon film is deposited on one side of the mica sheet, a gold film is deposited on the other side of the mica sheet, the side of the mica sheet deposited gold film is connected with the lower electrode, and the gas supply system is connected with the plasma processing chamber and supplies. The method is mainly used for preparing graphene.
Description
Technical Field
The invention belongs to the technical field of graphene preparation, and particularly relates to a device and a method for preparing dielectric barrier discharge graphene.
Background
The dielectric barrier discharge is used as a plasma discharge technology, atmospheric pressure discharge and material treatment can be realized, graphene is widely applied in various fields, various physical or chemical preparation methods of the graphene have advantages and disadvantages, and how to realize the preparation of the graphene under atmospheric pressure is a desire of material scientists. The chemical method for preparing the graphene at present has the problems of pollution, material defects and the like, the physical method for preparing the graphene generally needs a strict vacuum environment, the methods also have the defects of low yield, subsequent treatment and the like, and the preparation method has great restriction, so the application development of the graphene is limited. At present, the related research of oxidation reduction of graphene powder by using a dielectric barrier discharge technology exists, but the problems of tiling and stacking of prefabricated graphene powder and the like exist, and a graphene preparation device and a graphene preparation method capable of realizing industrial production are urgently needed in the application market.
Disclosure of Invention
The invention provides a device and a method for preparing dielectric barrier discharge graphene, aiming at solving the problems in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation device of dielectric barrier discharge graphene comprises a plasma processing chamber, a gas supply system, a power supply system and a detection and analysis system, wherein the plasma processing chamber adopts a horizontal flat capacitor combined dielectric barrier discharge structure, the plasma processing chamber comprises an upper electrode, a quartz medium, a mica sheet and a lower electrode, the upper electrode and the lower electrode are respectively connected with two ends of the power supply system, a discharge area is arranged between the upper electrode and the lower electrode, a palladium film is deposited on the surface of the quartz medium, the quartz medium is connected with the electrodes, a monomolecular carbon film is deposited on one side of the mica sheet, a gold film is deposited on the other side of the mica sheet, the gold film deposited side of the mica sheet is connected with the lower electrode, the gas supply system and the plasma processing chamber supply gas into the plasma processing chamber, and the detection and analysis system is connected with the plasma processing chamber and the power supply system, parameters of the power supply system and the discharge plasma in the plasma processing chamber are detected and analyzed.
Furthermore, the detection analysis system comprises a power supply detection subsystem and a spectrum analysis subsystem, wherein the power supply detection subsystem monitors parameters of the power supply system in real time, and the spectrum analysis subsystem carries out discharge spectrum analysis on discharge plasma in the plasma processing chamber and monitors a discharge state.
Furthermore, the power supply detection subsystem comprises an oscilloscope and a voltage probe, the oscilloscope is connected with the voltage probe, and the voltage probe is connected with the power supply system.
Furthermore, the spectrum analysis subsystem comprises an optical fiber probe, a spectrometer, an image sensor and a computer, wherein the optical fiber probe is arranged in the plasma processing chamber, and the optical fiber probe is sequentially connected with the spectrometer, the image sensor and the computer.
Furthermore, an electromagnetic element is arranged outside the upper electrode and the lower electrode.
Further, the gas supplied by the gas supply system into the plasma processing chamber is methane.
Furthermore, the upper electrode and the lower electrode are made of stainless steel materials.
Furthermore, one end of the power supply system is connected with the grounding electrode and the lower electrode.
Furthermore, a shielding box is arranged outside the power supply system.
The invention also provides a preparation method of the dielectric barrier discharge graphene, which comprises the following steps:
the method comprises the following steps: placing the prefabricated mica sheet deposited with the monomolecular carbon film into a dielectric barrier discharge area, starting a gas supply system, and continuously supplying methane gas to the discharge area in the plasma processing chamber;
step two: starting a power supply system to enable a discharge area to be bound in a discharge area between the upper electrode and the lower electrode, and switching on the electromagnetic element to improve the plasma density;
step three: the power system parameters are detected in real time by a power detection subsystem consisting of an oscilloscope and a voltage probe, the discharge plasma density and particles are subjected to discharge spectral analysis by a spectral analysis subsystem consisting of an optical fiber probe, a spectrometer, an image sensor and a computer, and the discharge state is monitored in the whole process;
step four: and preparing the carbon film into graphene, closing the electromagnetic element, the power supply system and the gas supply system in sequence, taking out the mica sheet, stripping the prepared graphene from the surface of the mica sheet, and finishing the treatment.
Compared with the prior art, the invention has the beneficial effects that: the invention solves the problems that the existing graphene preparation is difficult to be carried out under atmospheric pressure, and simultaneously has pollution and material defects.
Under the comprehensive actions of the catalysis of a palladium membrane, methane gas, an electromagnetic element and the like, the preparation and application of graphene are realized by utilizing dielectric barrier discharge to act on a monomolecular carbon membrane prefabricated on a mica sheet. The device and the method are purely physical modification, the preparation method is environment-friendly, the device is reasonable in structure, good in stability, good in repeatability of processing results, normal in temperature and pressure and high in production efficiency.
Drawings
Fig. 1 is a schematic structural diagram of a device for preparing dielectric barrier discharge graphene according to the present invention.
1-plasma processing chamber, 2-electromagnetic element, 3-gas supply system, 4-upper electrode, 5-quartz medium, 6-palladium film, 7-discharge area, 8-carbon film, 9-mica sheet, 10-gold film, 11-lower electrode, 12-shielding box, 13-power supply system, 14-oscilloscope, 15-optical fiber probe, 16-spectrometer, 17-image sensor, 18-computer, 19-voltage probe and 20-grounding electrode.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely explained below with reference to the drawings in the embodiments of the present invention.
Referring to fig. 1 to illustrate the present embodiment, a dielectric barrier discharge graphene preparation apparatus includes a plasma processing chamber 1, a gas supply system 3, a power supply system 13 and a detection analysis system, where the plasma processing chamber 1 adopts a horizontal flat capacitor combined dielectric barrier discharge structure, the plasma processing chamber 1 includes an upper electrode 4, a quartz medium 5, a mica sheet 9 and a lower electrode 11, the upper electrode 4 and the lower electrode 11 are respectively connected to two ends of the power supply system 13, a discharge region 7 is between the upper electrode 4 and the lower electrode 11, a palladium film 6 is deposited on the surface of the quartz medium 5, the quartz medium 5 is connected to the electrode 4, a monomolecular carbon film 8 is deposited on one side of the mica sheet 9, a gold film 10 is deposited on the other side of the mica sheet 9, the gold film 10 side of the mica sheet 9 is connected to the lower electrode 11, the gas supply system 3 is connected to the plasma processing chamber 1, and a detection and analysis system is connected with the plasma processing chamber 1 and the power supply system 13 and is used for detecting and analyzing parameters of the power supply system 13 and the discharge plasma in the plasma processing chamber 1.
In the embodiment, the surface of the quartz medium 5 is deposited with the thin palladium film 6 in advance by using a magnetron sputtering method, the mica sheet 9 is used as a carrier for preparing the graphene, the magnetron sputtering method is facilitated to deposit the thin gold film 10 on one side of the prefabricated mica sheet 9, the vapor deposition method is used to deposit the monomolecular carbon film 8 on the other side of the prefabricated mica sheet 9, and the graphene can be peeled from the mica sheet 9 after the preparation is completed. The upper electrode 4 and the lower electrode 11 are both made of stainless steel materials, and the gap of the discharge area 1 between the upper electrode 4 and the lower electrode 11 is adjustable. The electromagnetic elements 2 are arranged on the outer sides of the upper electrode 4 and the lower electrode 11, so that the plasma density is improved and the adjusting process is improved. A high-frequency high-voltage power supply is adopted as a discharge power supply system 13, one end of the power supply system 13 is connected with the upper electrode 4, and the other end of the power supply system is grounded and connected with the lower electrode 11. The shielding box 12 is provided outside the power supply system 13. The gas supply system 3 mainly controls the type and flow rate of gas supplied into the plasma processing chamber 1, and supplies 99.9% methane gas participating in graphene production into the plasma processing chamber 1. The detection and analysis system comprises a power supply detection subsystem and a spectrum analysis subsystem, wherein the power supply detection subsystem monitors parameters of a power supply system 13 in real time, the spectrum analysis subsystem carries out discharge spectrum analysis on the density of discharge plasma and particles in a plasma processing chamber 1, the whole process monitors the discharge state and guides the process, the power supply detection subsystem comprises an oscilloscope 14 and a voltage probe 19, the oscilloscope 14 is connected with the voltage probe 19, the voltage probe 19 is connected with the power supply system 13, the spectrum analysis subsystem comprises an optical fiber probe 15, a spectrometer 16, an image sensor 17 and a computer 18, the optical fiber probe 15 is arranged in the plasma processing chamber 1, and the optical fiber probe 15 is sequentially connected with the spectrometer 16, the image sensor 17 and the computer 18.
The invention also provides a preparation method of the dielectric barrier discharge graphene, which comprises the following steps:
the method comprises the following steps: placing the prefabricated mica sheet 9 deposited with the monomolecular carbon film 8 into the dielectric barrier discharge region 7, starting the gas supply system 3, and continuously supplying methane gas to the discharge region 7 in the plasma processing chamber 1;
step two: starting a high-frequency high-voltage power supply system 13 to enable a discharge area to be bounded in a discharge area 7 between an upper electrode 4 and a lower electrode 11, and switching on an electromagnetic element 2 to improve the plasma density;
step three: the parameters of the power supply system 13 are detected in real time by a power supply detection subsystem consisting of an oscilloscope 14 and a voltage probe 19, the discharge spectral analysis of the discharge plasma density, particles and the like is carried out by a spectral analysis subsystem consisting of an optical fiber probe 15, a spectrometer 16, an image sensor 17 and a computer 18, and the discharge state is monitored in the whole process;
step four: after the carbon film 8 is prepared into graphene, the electromagnetic element 2, the power supply system 13 and the gas supply system 3 are sequentially closed, the mica sheet 9 is taken out, the prepared graphene is peeled off from the surface of the mica sheet 9, and the treatment is completed.
The device and the method for preparing the dielectric barrier discharge graphene provided by the invention are described in detail, and the principle and the implementation mode of the invention are explained by applying specific examples, and the description of the examples is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. A dielectric barrier discharge graphene preparation device is characterized in that: the device comprises a plasma processing chamber (1), a gas supply system (3), a power supply system (13) and a detection and analysis system, wherein the plasma processing chamber (1) adopts a horizontal plate capacitor combined dielectric barrier discharge structure, the plasma processing chamber (1) comprises an upper electrode (4), a quartz medium (5), a mica sheet (9) and a lower electrode (11), the upper electrode (4) and the lower electrode (11) are respectively connected with two ends of the power supply system (13), a discharge area (7) is arranged between the upper electrode (4) and the lower electrode (11), a palladium film (6) is deposited on the surface of the quartz medium (5), the quartz medium (5) is connected with the electrode (4), a monomolecular carbon film (8) is deposited on one side of the mica sheet (9), a gold film (10) is deposited on the other side of the mica sheet (9), and the gold film (10) deposited side of the mica sheet (9) is connected with the lower electrode (11), the gas supply system (3) is connected with the plasma processing chamber (1) and supplies gas into the plasma processing chamber (1), and the detection and analysis system is connected with the plasma processing chamber (1) and the power supply system (13) and is used for detecting and analyzing parameters of the power supply system (13) and discharge plasma in the plasma processing chamber (1).
2. The device for preparing dielectric barrier discharge graphene according to claim 1, wherein: the detection and analysis system comprises a power supply detection subsystem and a spectrum analysis subsystem, wherein the power supply detection subsystem carries out real-time monitoring on parameters of a power supply system (13), and the spectrum analysis subsystem carries out discharge spectrum analysis on discharge plasma in the plasma processing chamber (1) and monitors a discharge state.
3. The device for preparing dielectric barrier discharge graphene according to claim 2, wherein: the power supply detection subsystem comprises an oscilloscope (14) and a voltage probe (19), the oscilloscope (14) is connected with the voltage probe (19), and the voltage probe (19) is connected with the power supply system (13).
4. The device for preparing dielectric barrier discharge graphene according to claim 2 or 3, wherein: the spectral analysis subsystem comprises an optical fiber probe (15), a spectrometer (16), an image sensor (17) and a computer (18), wherein the optical fiber probe (15) is arranged in the plasma processing chamber (1), and the optical fiber probe (15) is sequentially connected with the spectrometer (16), the image sensor (17) and the computer (18).
5. The device for preparing dielectric barrier discharge graphene according to claim 1, wherein: and electromagnetic elements (2) are arranged on the outer sides of the upper electrode (4) and the lower electrode (11).
6. The device for preparing dielectric barrier discharge graphene according to claim 1, wherein: the gas supplied by the gas supply system (3) into the plasma processing chamber (1) is methane.
7. The device for preparing dielectric barrier discharge graphene according to claim 1, wherein: the upper electrode (4) and the lower electrode (11) are both made of stainless steel materials.
8. The device for preparing dielectric barrier discharge graphene according to claim 1, wherein: one end of the power supply system (13) is connected with the grounding electrode (20) and the lower electrode (11).
9. The device for preparing dielectric barrier discharge graphene according to claim 1, wherein: and a shielding box (12) is arranged on the outer side of the power supply system (13).
10. The method for preparing the dielectric barrier discharge graphene as claimed in claim 1, wherein the method comprises the following steps: it comprises the following steps:
the method comprises the following steps: placing a prefabricated mica sheet (9) deposited with a monomolecular carbon film (8) into the dielectric barrier discharge region (7), starting the gas supply system (3), and continuously supplying methane gas to the discharge region (7) in the plasma processing chamber (1);
step two: a power supply system (13) is started, so that a discharge area is bounded in a discharge area (7) between an upper electrode (4) and a lower electrode (11), an electromagnetic element (2) is started, and the plasma density is improved;
step three: the parameters of the power supply system (13) are detected in real time by a power supply detection subsystem consisting of an oscilloscope (14) and a voltage probe (19), the discharge plasma density and particles are subjected to discharge spectral analysis by a spectral analysis subsystem consisting of an optical fiber probe (15), a spectrometer (16), an image sensor (17) and a computer (18), and the discharge state is monitored in the whole process;
step four: and preparing the carbon film (8) into graphene, closing the electromagnetic element (2), the power supply system (13) and the gas supply system (3) in sequence, taking out the mica sheet (9), stripping the prepared graphene from the surface of the mica sheet (9), and finishing the treatment.
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