Method for preparing graphene-based support membrane of transmission electron microscope grid by directly etching metal substrate

A metal substrate, transmission electron microscope technology, applied in the direction of material analysis, instruments, measurement devices, etc. using wave/particle radiation, can solve the problems of difficulty in obtaining single-layer or even few-layer graphene support films, difficulty in batch preparation, and high cost , to achieve the effect of high integrity, avoiding transfer process and low cost

Active Publication Date: 2017-06-20
PEKING UNIV
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Problems solved by technology

At present, the production methods of graphene support film include the following categories: 1. Transfer the mechanically peeled small graphene film to the transmission grid. This method is extremely inefficient, and it is difficult to obtain a single-layer or even a few-layer graphene support film.
2. Transfer the graphene film grown by chemical vapor deposition on copper foil to the transmission grid with the assistance of isopropanol. This method is costly and difficult to prepare in batches

Method used

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  • Method for preparing graphene-based support membrane of transmission electron microscope grid by directly etching metal substrate
  • Method for preparing graphene-based support membrane of transmission electron microscope grid by directly etching metal substrate
  • Method for preparing graphene-based support membrane of transmission electron microscope grid by directly etching metal substrate

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Embodiment 1

[0078] Example 1. Direct etching of copper foil substrate to produce graphene transmission net support film

[0079] Such as figure 1 Shown is a schematic flow diagram of the preparation method of the present invention, such as figure 2 Shown is the overall concept of the preparation method of the present invention. The specific implementation process is as follows:

[0080] 1) The growth of graphene on a copper foil substrate uses a low pressure chemical vapor deposition system (LPCVD). The copper foil (purity 99.8%, thickness 25mm) is annealed in a hydrogen atmosphere for 30 minutes at 1000℃, the hydrogen flow rate is 300sccm, the system pressure is maintained at 350Pa, and then annealed in an argon atmosphere for 30 minutes, the argon flow rate is 500sccm , The system pressure is maintained at 500Pa. The effect of annealing under hydrogen atmosphere is to reduce the oxide layer on the surface of the copper foil, and the effect of annealing under argon atmosphere is to reduce ...

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Abstract

The invention discloses a method for preparing a graphene-based support membrane of a transmission electron microscope grid by directly etching a metal substrate. The method comprises the following steps: (1) growing graphene on the surface of a metal substrate by a chemical vapor deposition method; (2) removing the graphene growing on the back of the metal substrate; (3) preparing a polymer fiber network on the surface of the graphene to form a metal substrate/graphene/polymer fiber network structure; (4) preparing a cyclic pattern on the back of the metal substrate by a photoetching method; and (5) removing the metal substrate exposed out of the cyclic pattern by an etching method, and then removing the cyclic pattern. The preparation method disclosed by the invention avoids the transfer process of the graphene and does not need an extra transmission grid, and can obtain a copper grid and the graphene support membrane meeting the sample preparation requirements of a transmission electron microscope through one-step etching; thus, high efficiency, low cost, and batch preparation can be achieved.

Description

Technical field [0001] The invention relates to a method for directly etching a metal substrate to prepare a graphene-based transmission electron microscope supporting film. Background technique [0002] Graphene is composed of a single layer of carbon atoms with sp 2 The two-dimensional material formed by hybridization has stable physical and chemical properties, excellent mechanical strength, and excellent electrical and thermal conductivity. It can block all molecules, atoms and ions except protons. It is an excellent support, encapsulation and The barrier layer material is extremely suitable for making high-resolution transmission electron microscope support film. Compared with the traditional amorphous carbon film support film (thickness is usually greater than 3 nanometers), the ultra-flat, ultra-thin, atomic-thick graphene support film with good conductivity is expected to further improve the spatial resolution of the transmission electron microscope. The current producti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/22
CPCG01N23/2202
Inventor 党文辉彭海琳郑黎明邓兵
Owner PEKING UNIV
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