WO2021195995A1 - 一种介质阻挡放电石墨烯制备装置及制备方法 - Google Patents

一种介质阻挡放电石墨烯制备装置及制备方法 Download PDF

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WO2021195995A1
WO2021195995A1 PCT/CN2020/082530 CN2020082530W WO2021195995A1 WO 2021195995 A1 WO2021195995 A1 WO 2021195995A1 CN 2020082530 W CN2020082530 W CN 2020082530W WO 2021195995 A1 WO2021195995 A1 WO 2021195995A1
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supply system
discharge
power supply
dielectric barrier
processing chamber
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PCT/CN2020/082530
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English (en)
French (fr)
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张波
金旭栋
虞文武
马雯雯
高之涵
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常州机电职业技术学院
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Priority to PCT/CN2020/082530 priority Critical patent/WO2021195995A1/zh
Publication of WO2021195995A1 publication Critical patent/WO2021195995A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • C01B32/186—Preparation by chemical vapour deposition [CVD]
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma

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  • the invention belongs to the technical field of graphene preparation, and particularly relates to a dielectric barrier discharge graphene preparation device and a preparation method.
  • dielectric barrier discharge can achieve atmospheric pressure discharge and material processing.
  • Graphene has been widely used in various fields.
  • Various physical or chemical preparation methods of graphene have their own advantages and disadvantages. How to achieve it under atmospheric pressure
  • the preparation of graphene has always been a dream desire of materials scientists.
  • the chemical method of preparing graphene has problems such as pollution and material defects.
  • the physical method of preparing graphene generally requires a strict vacuum environment. These methods also have disadvantages such as low yield and need for subsequent processing, and there are great preparation methods. Therefore, the application and development of graphene are restricted.
  • the present invention proposes a dielectric barrier discharge graphene preparation device and a preparation method.
  • a dielectric barrier discharge graphene preparation device which includes a plasma processing chamber, a gas supply system, a power supply system, and a detection and analysis system.
  • the plasma processing chamber adopts a horizontal flat plate. Capacitor combined with a dielectric barrier discharge structure.
  • the plasma processing chamber includes an upper electrode, a quartz medium, a mica sheet, and a lower electrode. The upper electrode and the lower electrode are respectively connected to both ends of the power supply system.
  • the palladium film is deposited on the surface of the quartz medium, the quartz medium is connected to the electrode, the monomolecular carbon film is deposited on one side of the mica sheet, the gold film is deposited on the other side, and the gold film side is deposited on the mica sheet
  • the gas supply system is connected to the plasma processing chamber to supply gas into the plasma processing chamber
  • the detection and analysis system is connected to the plasma processing chamber and the power supply system, and the parameters of the power supply system and the plasma processing chamber Discharge plasma for detection and analysis.
  • the detection and analysis system includes a power detection subsystem and a spectrum analysis subsystem.
  • the power detection subsystem monitors the parameters of the power system in real time.
  • the spectrum analysis subsystem monitors the discharge plasma in the plasma processing chamber. Perform discharge spectrum analysis and monitor the discharge status.
  • the power detection subsystem includes an oscilloscope and a voltage probe, the oscilloscope is connected to the voltage probe, and the voltage probe is connected to the power supply system.
  • the spectrum analysis subsystem includes an optical fiber probe, a spectrometer, an image sensor, and a computer.
  • the optical fiber probe is arranged in the plasma processing chamber, and the optical fiber probe is connected to the spectrometer, the image sensor, and the computer in sequence.
  • electromagnetic elements are arranged outside the upper electrode and the lower electrode.
  • the gas supplied by the gas supply system to the plasma processing chamber is methane.
  • the upper electrode and the lower electrode are made of stainless steel.
  • one end of the power supply system is connected to the ground electrode and the lower electrode.
  • a shielding box is provided on the outside of the power supply system.
  • the present invention also provides a method for preparing dielectric barrier discharge graphene, which includes the following steps:
  • Step 1 Put the prefabricated mica sheet on which the monomolecular carbon film is deposited into the dielectric barrier discharge area, start the gas supply system, and continue to supply methane gas to the discharge area in the plasma processing chamber;
  • Step 2 Turn on the power system, make the discharge area bound to the discharge area between the upper electrode and the lower electrode, turn on the electromagnetic element, and increase the plasma density;
  • Step 3 Perform real-time detection of power supply system parameters through the power detection subsystem composed of oscilloscope and voltage probe, and perform discharge spectrum analysis on the discharge plasma density and particles through the spectrum analysis subsystem composed of optical fiber probe, spectrometer, image sensor and computer. Monitor the discharge status during the whole process;
  • Step 4 After preparing the carbon film into graphene, turn off the electromagnetic element, power supply system and gas supply system in turn, take out the mica sheet, peel off the prepared graphene from the surface of the mica sheet, and the processing is completed.
  • the present invention Compared with the prior art, the present invention has the beneficial effects that: the present invention solves the problems that the existing graphene preparation is difficult to be carried out under atmospheric pressure, and there are problems of pollution and material defects at the same time.
  • the invention utilizes the dielectric barrier discharge to act on the monomolecular carbon film prefabricated on the mica sheet under the comprehensive effects of the catalysis of the palladium film, methane gas and electromagnetic elements, and realizes the preparation and application of graphene.
  • the device and method are purely modified by physical methods, the preparation method is environmentally friendly, the device structure is reasonable, the stability is good, the processing results are good repeatability, the normal temperature and pressure, and the production efficiency is high.
  • Fig. 1 is a schematic diagram of the structure of a dielectric barrier discharge graphene preparation device according to the present invention.
  • 1-plasma processing chamber 2-electromagnetic element, 3-gas supply system, 4-upper electrode, 5-quartz medium, 6-palladium membrane, 7-discharge area, 8-carbon membrane, 9-mica sheet, 10- Gold film, 11-lower electrode, 12-shielded box, 13-power supply system, 14-oscilloscope, 15-fiber probe, 16-spectrometer, 17-image sensor, 18-computer, 19-voltage probe, 20-ground electrode.
  • a dielectric barrier discharge graphene preparation device which includes a plasma processing chamber 1, a gas supply system 3, a power supply system 13, and a detection and analysis system.
  • the plasma processing chamber 1 adopts a horizontal flat plate. Capacitor combined with a 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 connected to both ends of the power supply system 13, respectively, A discharge area 7 is formed 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, and a monomolecular carbon film is deposited on one side of the mica sheet 9 8.
  • the gold film 10 is deposited on the other side, the gold film 10 side of the mica sheet 9 is connected to the bottom electrode 11, the gas supply system 3 is connected to the plasma processing chamber 1, and gas is supplied into the plasma processing chamber 1, so
  • the detection and analysis system is connected to the plasma processing chamber 1 and the power supply system 13 to detect and analyze the parameters of the power supply system 13 and the discharge plasma in the plasma processing chamber 1.
  • a thin layer of palladium film 6 is deposited on the surface of the quartz medium 5 by magnetron sputtering in advance, and the mica sheet 9 is used as a carrier for preparing graphene, which facilitates the magnetron sputtering method to deposit a thin layer of gold film on one side of the prefabricated mica sheet 9 10.
  • the graphene After the graphene is prepared, it can be peeled from the mica sheet 9.
  • the upper electrode 4 and the lower electrode 11 are made of stainless steel, and the gap of the discharge area 1 between the upper electrode 4 and the lower electrode 11 is adjustable.
  • Electromagnetic elements 2 are arranged outside the upper electrode 4 and the lower electrode 11 to improve the plasma density and adjust the process.
  • a high-frequency and high-voltage power supply is used as the discharge power supply system 13, one end of the power supply system 13 is connected to the upper electrode 4, and the other end is grounded and connected to the lower electrode 11.
  • a shielding box 12 is provided outside the power supply system 13.
  • the gas supply system 3 mainly controls the supply of the gas type and flow rate entering the plasma processing chamber 1, and supplies 99.9% methane gas that participates in the preparation of graphene into the plasma processing chamber 1.
  • the detection and analysis system includes a power detection subsystem and a spectrum analysis subsystem. The power detection subsystem monitors the parameters of the power system 13 in real time.
  • the spectrum analysis subsystem discharges the discharge plasma density and particles in the plasma processing chamber 1 Spectral analysis, monitoring the discharge status and guiding the process in the whole process, the power detection subsystem includes an oscilloscope 14 and a voltage probe 19, the oscilloscope 14 is connected to the voltage probe 19, the voltage probe 19 is connected to the power system 13, and the spectrum analysis subsystem includes an optical fiber probe 15 , The spectrometer 16, the image sensor 17, and the computer 18. The optical fiber probe 15 is arranged in the plasma processing chamber 1, and the optical fiber probe 15 is connected to the spectrometer 16, the image sensor 17 and the computer 18 in sequence.
  • the present invention also provides a method for preparing dielectric barrier discharge graphene, which includes the following steps:
  • Step 1 Put the prefabricated mica sheet 9 on which the monomolecular carbon film 8 is deposited into the dielectric barrier discharge area 7, start the gas supply system 3, and continue to supply methane gas to the discharge area 7 in the plasma processing chamber 1;
  • Step 2 Turn on the high-frequency and high-voltage power supply system 13, so that the discharge area is bound to the discharge area 7 between the upper electrode 4 and the lower electrode 11, and the electromagnetic element 2 is turned on to increase the plasma density;
  • Step 3 Real-time detection of the parameters of the power supply system 13 through the power detection subsystem composed of the oscilloscope 14 and the voltage probe 19, and the spectral analysis subsystem composed of the optical fiber probe 15, the spectrometer 16, the image sensor 17 and the computer 18 to measure the discharge plasma density Perform discharge spectrum analysis with particles, etc., and monitor the discharge status in the whole process;
  • Step 4 After preparing the carbon film 8 into graphene, turn off the electromagnetic element 2, the power supply system 13 and the gas supply system 3 in turn, take out the mica sheet 9 and peel off the prepared graphene from the surface of the mica sheet 9, and the processing is completed.

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Abstract

本发明提出了一种介质阻挡放电石墨烯制备装置及制备方法，属于石墨烯制备技术领域。解决了现有石墨烯的制备难以在大气压下进行，同时存在污染和材料缺陷的问题。它包括等离子体处理室、气体供给系统、电源系统和检测分析系统，等离子体处理室采用卧式平板电容结合介质阻挡放电的结构，等离子体处理室包括上电极、石英介质、云母片和下电极，上电极和下电极分别与电源系统两端相连，上电极和下电极之间为放电区域，石英介质表面沉积有钯膜，石英介质与电极相连，云母片一侧沉积单分子碳膜，另一侧沉积金膜，云母片沉积金膜侧与下电极相连，气体供给系统与等离子体处理室，向等离子体处理室内供给气体。它主要用于石墨烯的制备。

Description

一种介质阻挡放电石墨烯制备装置及制备方法 技术领域
本发明属于石墨烯制备技术领域，特别是涉及一种介质阻挡放电石墨烯制备装置及制备方法。
背景技术
介质阻挡放电作为一种等离子体放电技术，可以实现大气压放电及材料处理，石墨烯在各领域得到了广泛应用，石墨烯的各种物理或化学等制备方法各有优缺点，如何在大气压下实现石墨烯的制备一直是材料科学家梦寐以求的愿望。目前化学方法制备石墨烯存在污染和材料存在缺陷等问题，物理方法制备石墨烯一般都需要严格的真空环境，这些方法制备也存在产率不高、需要后续处理等缺点，制备方法上存在很大的制约，因此限制了石墨烯的应用发展。目前也存在利用介质阻挡放电技术对石墨烯粉体进行氧化还原的相关研究，但存在预制石墨烯粉体平铺堆积等问题，应用市场上急需一种能实现产业化生产的石墨烯制备装置及制备方法。
发明内容
本发明为了解决现有技术中的问题，提出一种介质阻挡放电石墨烯制备装置及制备方法。
为实现上述目的，本发明采用以下技术方案：一种介质阻挡放电石墨烯制备装置，它包括等离子体处理室、气体供给系统、电源系统和检测分析系统，所述等离子体处理室采用卧式平板电容结合介质阻挡放电的结构，所述等离子体处理室包括上电极、石英介质、云母片和下电极，所述上电极和下电极分别与电源系统两端相连，所述上电极和下电极之间为放电区域，所述石英介质表面沉积有钯膜，所述石英介质与电极相连，所述云母片一侧沉积单分子碳膜，另一侧沉积金膜，所述云母片沉积金膜侧与下电极相连，所述气体供给系统与等离子体处理室，向等离子体处理室内供给气体，所述检测分析系统与等离子体处理室和电源系统相连，对电源系统的参数及等离子体处理室内的放电等离子体进行检测和分析。
更进一步的，所述检测分析系统包括电源检测子系统和光谱分析子系统，所述电源检测子系统对电源系统的参数进行实时监测，所述光谱分析子系统对等离子体处理室内的放电等离子体进行放电光谱分析并监测放电状态。
更进一步的，所述电源检测子系统包括示波器和电压探头，所述示波器与电压探头相连，所述电压探头与电源系统相连。
更进一步的，所述光谱分析子系统包括光纤探头、光谱仪、图像传感器和计算机，所述光纤探头设置在等离子体处理室内，所述光纤探头与光谱仪、图像传感器和计算机依次相连。
更进一步的，所述上电极和下电极外侧设置有电磁元件。
更进一步的，所述气体供给系统向等离子体处理室内供给的气体为甲烷。
更进一步的，所述上电极和下电极均为不锈钢材料。
更进一步的，所述电源系统一端与接地电极和下电极相连。
更进一步的，所述电源系统外侧设置有屏蔽箱。
本发明还提供了一种介质阻挡放电石墨烯的制备方法，它包括以下步骤：
步骤一：将沉积沉积单分子碳膜的预制云母片放入介质阻挡放电区域，启动气体供给系统，持续向等离子体处理室内放电区域供给甲烷气体；
步骤二：开启电源系统，使放电区束缚在上电极和下电极之间的放电区域，开通电磁元件，提高等离子体密度；
步骤三：通过示波器和电压探头组成的电源检测子系统对电源系统参数进行实时检测，通过光纤探头、光谱仪、图像传感器和计算机组成的光谱分析子系统对放电等离子体密度和粒子进行放电光谱分析，全过程监测放电状态；
步骤四：将碳膜备成石墨烯后，依次关闭电磁元件、电源系统和气体供给系统，取出云母片，从云母片表面剥离制备好的石墨烯，处理完成。
与现有技术相比，本发明的有益效果是：本发明解决了现有石墨烯的制备难以在大气压下进行，同时存在污染和材料缺陷的问题。
本发明在钯膜的催化、甲烷气体和电磁元件等综合作用下，利用介质阻挡放电作用于云母片上预制的单分子碳膜，实现石墨烯制备和应用。该装置和方法为纯物理方法改性、制备方法环保，装置结构合理、稳定性好、处理结果重复性好，常温常压、生产效率高。
附图说明
图1为本发明所述的一种介质阻挡放电石墨烯制备装置结构示意图。
1-等离子体处理室，2-电磁元件，3-气体供给系统，4-上电极，5-石英介质，6-钯膜，7-放电区域，8-碳膜，9-云母片，10-金膜，11-下电极，12-屏蔽箱，13-电源系统，14-示波器，15-光纤探头，16-光谱仪，17-图像传感器，18-计算机，19-电压探头，20-接地电极。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地 阐述。
参见图1说明本实施方式，一种介质阻挡放电石墨烯制备装置，它包括等离子体处理室1、气体供给系统3、电源系统13和检测分析系统，所述等离子体处理室1采用卧式平板电容结合介质阻挡放电的结构，所述等离子体处理室1包括上电极4、石英介质5、云母片9和下电极11，所述上电极4和下电极11分别与电源系统13两端相连，所述上电极4和下电极11之间为放电区域7，所述石英介质5表面沉积有钯膜6，所述石英介质5与电极4相连，所述云母片9一侧沉积单分子碳膜8，另一侧沉积金膜10，所述云母片9沉积金膜10侧与下电极11相连，所述气体供给系统3与等离子体处理室1，向等离子体处理室1内供给气体，所述检测分析系统与等离子体处理室1和电源系统13相连，对电源系统13的参数及等离子体处理室1内的放电等离子体进行检测和分析。
本实施例石英介质5表面提前利用磁控溅射法沉积薄层钯膜6，云母片9作为制备石墨烯的载体，利于磁控溅射法在预制云母片9的一侧沉积薄层金膜10，利用气相沉积法在预制云母片9的另一侧沉积单分子碳膜8，石墨烯制备完成后，可以从云母片9剥离。上电极4和下电极11均为不锈钢材料，上电极4和下电极11间的放电区域1间隙可调。上电极4和下电极11外侧设置有电磁元件2，提高等离子体密度和调节工艺。采用高频高压电源作为放电电源系统13，电源系统13一端连接上电极4，另一端接地并与下电极11相连。电源系统13外侧设置有屏蔽箱12。气体供给系统3主要控制进入等离子体处理室1的气体类型和流量的供给，向等离子体处理室1内供给参与石墨烯制备的为99.9％的甲烷气体。检测分析系统包括电源检测子系统和光谱分析子系统，电源检测子系统对电源系统13的参数进行实时监测，光谱分析子系统对等离子体处理室1内的放电等离子体密度和粒子等进进行放电光谱分析，全过程监测放电状态和指导工艺过程，电源检测子系统包括示波器14和电压探头19，示波器14与电压探头19相连，电压探头19与电源系统13相连，光谱分析子系统包括光纤探头15、光谱仪16、图像传感器17和计算机18，光纤探头15设置在等离子体处理室1内，光纤探头15与光谱仪16、图像传感器17和计算机18依次相连。
本发明还提供了一种介质阻挡放电石墨烯的制备方法，它包括以下步骤：
步骤一：将沉积沉积单分子碳膜8的预制云母片9放入介质阻挡放电区域7，启动气体供给系统3，持续向等离子体处理室1内放电区域7供给甲烷气体；
步骤二：开启高频高压电源系统13，使放电区束缚在上电极4和下电极11之间的放电区域7，开通电磁元件2，提高等离子体密度；
步骤三：通过示波器14和电压探头19组成的电源检测子系统对电源系统13参数进行实时检测，通过光纤探头15、光谱仪16、图像传感器17和计算机18组成的光谱分析子系统对放电等离子体密度和粒子等进行放电光谱分析，全过程监测放电状态；
步骤四：将碳膜8备成石墨烯后，依次关闭电磁元件2、电源系统13和气体供给系统3，取出云母片9，从云母片9表面剥离制备好的石墨烯，处理完成。
以上对本发明所提供的一种介质阻挡放电石墨烯制备装置及制备方法，进行了详细介绍，本文中应用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的一般技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处，综上所述，本说明书内容不应理解为对本发明的限制。

Claims (10)

  1. 一种介质阻挡放电石墨烯制备装置，其特征在于：它包括等离子体处理室(1)、气体供给系统(3)、电源系统(13)和检测分析系统，所述等离子体处理室(1)采用卧式平板电容结合介质阻挡放电的结构，所述等离子体处理室(1)包括上电极(4)、石英介质(5)、云母片(9)和下电极(11)，所述上电极(4)和下电极(11)分别与电源系统(13)两端相连，所述上电极(4)和下电极(11)之间为放电区域(7)，所述石英介质(5)表面沉积有钯膜(6)，所述石英介质(5)与电极(4)相连，所述云母片(9)一侧沉积单分子碳膜(8)，另一侧沉积金膜(10)，所述云母片(9)沉积金膜(10)侧与下电极(11)相连，所述气体供给系统(3)与等离子体处理室(1)，向等离子体处理室(1)内供给气体，所述检测分析系统与等离子体处理室(1)和电源系统(13)相连，对电源系统(13)的参数及等离子体处理室(1)内的放电等离子体进行检测和分析。
  2. 根据权利要求1所述的一种介质阻挡放电石墨烯制备装置，其特征在于：所述检测分析系统包括电源检测子系统和光谱分析子系统，所述电源检测子系统对电源系统(13)的参数进行实时监测，所述光谱分析子系统对等离子体处理室(1)内的放电等离子体进行放电光谱分析并监测放电状态。
  3. 根据权利要求2所述的一种介质阻挡放电石墨烯制备装置，其特征在于：所述电源检测子系统包括示波器(14)和电压探头(19)，所述示波器(14)与电压探头(19)相连，所述电压探头(19)与电源系统(13)相连。
  4. 根据权利要求2或3所述的一种介质阻挡放电石墨烯制备装置，其特征在于：所述光谱分析子系统包括光纤探头(15)、光谱仪(16)、图像传感器(17)和计算机(18)，所述光纤探头(15)设置在等离子体处理室(1)内，所述光纤探头(15)与光谱仪(16)、图像传感器(17)和计算机(18)依次相连。
  5. 根据权利要求1所述的一种介质阻挡放电石墨烯制备装置，其特征在于：所述上电极(4)和下电极(11)外侧设置有电磁元件(2)。
  6. 根据权利要求1所述的一种介质阻挡放电石墨烯制备装置，其特征在于：所述气体供给系统(3)向等离子体处理室(1)内供给的气体为甲烷。
  7. 根据权利要求1所述的一种介质阻挡放电石墨烯制备装置，其特征在于：所述上电极(4)和下电极(11)均为不锈钢材料。
  8. 根据权利要求1所述的一种介质阻挡放电石墨烯制备装置，其特征在于：所述电源系统(13)一端与接地电极(20)和下电极(11)相连。
  9. 根据权利要求1所述的一种介质阻挡放电石墨烯制备装置，其特征在于：所述电源 系统(13)外侧设置有屏蔽箱(12)。
  10. 一种如权利要求1所述的介质阻挡放电石墨烯制备装置的制备方法，其特征在于：它包括以下步骤：
    步骤一：将沉积沉积单分子碳膜(8)的预制云母片(9)放入介质阻挡放电区域(7)，启动气体供给系统(3)，持续向等离子体处理室(1)内放电区域(7)供给甲烷气体；
    步骤二：开启电源系统(13)，使放电区束缚在上电极(4)和下电极(11)之间的放电区域(7)，开通电磁元件(2)，提高等离子体密度；
    步骤三：通过示波器(14)和电压探头(19)组成的电源检测子系统对电源系统(13)参数进行实时检测，通过光纤探头(15)、光谱仪(16)、图像传感器(17)和计算机(18)组成的光谱分析子系统对放电等离子体密度和粒子进行放电光谱分析，全过程监测放电状态；
    步骤四：将碳膜(8)备成石墨烯后，依次关闭电磁元件(2)、电源系统(13)和气体供给系统(3)，取出云母片(9)，从云母片(9)表面剥离制备好的石墨烯，处理完成。
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