A kind of porous transmission electron microscope support film and ultra-flat graphene electron microscope grid and preparation method thereof
A technology of transmission electron microscopy and support film, which is applied in the fields of material analysis using radiation, material analysis using radiation diffraction, material analysis using wave/particle radiation, etc. It can solve immature preparation technology, unfavorable practical application, and graphene damage and other issues, to achieve the effect of controllable material and thickness, high-resolution imaging, and high integrity
Active Publication Date: 2022-04-26
PEKING UNIV
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Problems solved by technology
However, both of these two processes have a common deficiency: the growth substrate of graphene used is foil (copper foil, copper-nickel alloy, etc.), and there are a large number of steps, calendering lines, etc. on the surface of the foil, so the growth of graphene During the process, graphene will replicate the rough structure of the substrate, and there will be a large number of wrinkles on the surface
Among them, the porous support membrane with a circular hole array structure is still dependent on imports in my country, and the preparation technology is still immature in China
Moreover, when graphene is transferred using commercial porous support membranes on the market, it is easy to cause serious damage to graphene, which is not conducive to practical application.
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Embodiment 1
[0059] 1) Preparation of porous gold film: On a silicon template with a large-area circular hole array (the diameter of a single circular hole is 1.2 μm, and the depth of the circular hole groove is 0.5-5 μm), a layer is sequentially coated using a thermal evaporation vacuum coater. 20nm thick water-soluble sacrificial layer sodium metaphosphate and 20nm thick porous gold film, the vacuum degree is 5×10 -4 Pa, the coating rate is Then clamp a corner of the template, and slowly immerse the template in water at an inclination angle of 45°. After immersion in water, sodium metaphosphate dissolves rapidly, and the porous gold membrane is separated from the template at a separation speed of 0.1cm / s. After the template is completely submerged, the porous membrane will Float completely on the water surface, then recover the template, ultrasonically clean it in water, acetone, and isopropanol for 10 minutes, dry it and store it cleanly for the next use.
[0060] 2) Preparation of go...
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Abstract
The invention discloses a transmission electron microscope support film with a circular hole array structure, an ultra-flat graphene grid and a preparation method thereof. The method includes sequentially plating a water-soluble sacrificial layer and a porous electron microscope support film on a circular hole array template by vacuum coating, and making the porous support film float on the liquid surface by utilizing the water solubility of the sacrifice layer. Then, the porous support membrane is picked up with a commercial carrier net, and the composite structure of the porous film-carrier net is obtained after drying. Based on this, the ultra-flat graphene is transferred to the porous membrane by clean transfer to obtain the ultra-flat graphene grid. This method solves the technical problem of being stuck in the support membrane of the circular hole array electron microscope in China. The yield rate of the porous electron microscope support membrane is high, the aperture and thickness of the circular pores are controllable, and large-area preparation can be realized. At the same time, the ultra-flat graphene grid prepared by the invention has basically no wrinkles on the graphene surface, high mechanical strength, and a completeness of more than 98%. In addition, the surface of graphene is clean and free of pollutants, which is conducive to improving the imaging quality.
Description
technical field [0001] The invention belongs to the field of materials, and relates to a porous transmission electron microscope support film, an ultra-flat graphene electron microscope carrier network and a preparation method thereof. Background technique [0002] Graphene is an ideal grid material for transmission electron microscopy. Regularly arranged carbon monoatomic layers hardly introduce background interference to electron microscopy characterization, and can even provide extremely high contrast for single atoms and small organic molecules. and other fields have good application prospects. In addition, when graphene is used for high-resolution structural analysis of biomacromolecules under cryo-electron microscopy, it can effectively avoid the structural damage of biomacromolecules caused by the gas-liquid interface, and reduce the sample displacement caused by electron beam irradiation, which is conducive to improving the imaging quality. [0003] There are two ma...
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IPC IPC(8): G01N23/04G01N23/20G01N23/20008
CPCG01N23/04G01N23/20G01N23/20008
Inventor 彭海琳高啸寅郑黎明姚雅婷李天然
Owner PEKING UNIV