Preparation method of graphene film by virtue of normal-pressure chemical vapor deposition

A normal pressure chemical vapor phase, graphene film technology, applied in gaseous chemical plating, metal material coating process, coating and other directions, can solve problems such as difficulty in crystal domain control, affecting the quality of graphene film, etc., and achieve simple and convenient control. , easy to operate, simple steps

Active Publication Date: 2015-04-08
CHONGQING INST OF GREEN & INTELLIGENT TECH CHINESE ACADEMY OF SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a method for preparing a graphene film by atmospheric pressure chemical vapor deposi

Method used

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  • Preparation method of graphene film by virtue of normal-pressure chemical vapor deposition
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  • Preparation method of graphene film by virtue of normal-pressure chemical vapor deposition

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Embodiment 1

[0036] grow single-layer graphene films, such as image 3 As shown, the Raman spectrum of the grown single-layer graphene film, I 2D Peak and I G The ratio of the peaks is significantly greater than 1, indicating a single-layer graphene film. First, the copper foil with a length and width of 5 cm was cleaned with ethanol and acetone by ultrasonic cleaning for 20 minutes, and then cleaned in dilute nitric acid for 2 minutes to complete the cleaning of the copper foil. Then put the copper foil into the CVD tube furnace, under the condition of normal pressure, the H 2and Ar, the copper foil was heated to a temperature of 1000 °C in the mixed gas, and kept for annealing for 60 minutes. After the annealing of the copper foil is completed, the graphene nucleation is carried out, and the H 2 and Ar, while also passing 1sccm of CH 4 , holding time for 5 minutes, graphene nucleates to form graphene crystal domains. After the graphene crystal domains are formed, the copper foil is...

Embodiment 2

[0038] grow bilayer graphene films, such as Figure 4 As shown, the Raman spectrum of the grown double-layer graphene film, I 2D Peak and I G The peaks are almost at the same height, indicating a bilayer graphene film. First, the copper foil with a length and width of 5 cm was cleaned with ethanol and acetone by ultrasonic cleaning for 20 minutes, and then cleaned in dilute nitric acid for 2 minutes to complete the cleaning of the copper foil. Then put the copper foil into the CVD tube furnace, under the condition of normal pressure, the H 2 and Ar, the copper foil was heated to a temperature of 1000 °C in the mixed gas, and kept for annealing for 60 minutes. After the annealing of the copper foil is completed, the graphene nucleation is carried out, and the H 2 and Ar, while also passing 1sccm of CH 4 , holding time for 5 minutes, graphene nucleates to form graphene crystal domains. After the graphene crystal domains are formed, the copper foil is cooled to below 200°C,...

Embodiment 3

[0040] First, the copper foil with a length and width of 5 cm was cleaned with ethanol and acetone by ultrasonic cleaning for 20 minutes, and then cleaned in dilute nitric acid for 2 minutes to complete the cleaning of the copper foil. Then put the copper foil into the CVD tube furnace, under normal pressure conditions, the flow rate of 100 sccm and 200 sccm H 2 and Ar, the copper foil was heated to a temperature of 900 °C in the mixed gas, and kept for annealing for 60 minutes. After the annealing of the copper foil is completed, the graphene nucleation is carried out, and the H 2 and Ar, while also passing 0.1sccm of CH 4 , holding time for 20 minutes, graphene nucleates to form graphene crystal domains. After the graphene crystal domains are formed, the copper foil is cooled to below 200°C, then taken out from the CVD tube furnace, and the copper foil is heated in an environment with a temperature of 150°C for 1 minute, so that the copper foil that does not grow graphene ...

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Abstract

The invention relates to a preparation method of a graphene film by virtue of normal-pressure chemical vapor deposition in the technical field of graphene preparation and in particular relates to a sub-step preparation method of the graphene film controllable in crystal domain by virtue of normal-pressure chemical vapor deposition. The method comprises the following steps: 1) cleaning a metal substrate copper foil; 2) performing annealing treatment on the metal substrate copper foil; 3) performing graphene nucleation on the annealed copper foil to form a graphene crystal domain; 4) inerting the copper foil after the graphene nucleation; 5) melting down the inerted copper foil for growing and growing the graphene film from the graphene crystal domain; and 6) cooling the graphene film, thereby finishing the preparation of the graphene film. The preparation method of the graphene film by virtue of normal-pressure chemical vapor deposition has the beneficial effects of simple steps, convenient operations, and simple and convenient control on the density, size and number of layers of the graphene crystal domain by regulating the flow of the gas carbon source of the graphene at the nucleation stage, and consequently, the high-quality graphene film is formed.

Description

technical field [0001] The invention relates to a method for preparing a graphene film by atmospheric pressure chemical vapor deposition in the technical field of graphene preparation, in particular to a step-by-step preparation method for a controllable crystal domain by chemical vapor deposition of graphene film at atmospheric pressure. Background technique [0002] Graphene is a hexagonal honeycomb structure composed of carbon atoms based on sp2 hybridization, a two-dimensional crystal with a thickness of only one atomic layer. In 2004, Andre Geim, Konstantin Novoselov and others discovered stable single-layer graphene, and also won the 2010 Nobel Prize in Physics for their pioneering work on graphene. In recent years, graphene has shown many exciting properties and potential application prospects in the fields of microelectronics, quantum physics, materials, chemistry, etc., and has attracted extensive attention from the scientific and industrial circles. Graphene has e...

Claims

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Application Information

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IPC IPC(8): C23C16/453C23C16/26
CPCC23C16/26C23C16/453
Inventor 高翾黄德萍李占成张永娜朱鹏姜浩史浩飞杜春雷
Owner CHONGQING INST OF GREEN & INTELLIGENT TECH CHINESE ACADEMY OF SCI
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