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A method for realizing high-efficiency liquid encapsulation

A technology for liquid and liquid encapsulation, which is used in measurement devices, preparation of test samples, discharge tubes, etc., and can solve the problems of limited strength of silicon nitride, reduced imaging resolution, reduced liquid sealing efficiency and repeatability, etc.

Active Publication Date: 2019-06-18
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Earlier, the in-situ characterization of liquid phase reactions under transmission electron microscopy mostly relied on silicon nitride materials prepared by traditional silicon processes as encapsulation films. Due to the limited strength of silicon nitride, the film thickness required to achieve self-support, especially to support liquid bubbles, is often close to Hundreds of nanometers, greatly reducing the resolution of imaging
In addition, it has also been reported that the in situ characterization of the reaction relies on an open liquid pool, but most of the samples are ionic liquids with low saturated vapor pressure, which greatly limits the types of reaction systems that can be characterized.
There have been a few reports on the use of graphene films to encapsulate liquids in recent years, but limited by the quality of graphene and the encapsulation process, the types of liquids that can be encapsulated are limited, and the bubble size and density are also low, which greatly reduces the efficiency and repeatability of liquid sealing.

Method used

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  • A method for realizing high-efficiency liquid encapsulation
  • A method for realizing high-efficiency liquid encapsulation
  • A method for realizing high-efficiency liquid encapsulation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Example 1. High-efficiency packaging of high-quality graphene transmission grids in aqueous solution of gold nanoparticles

[0081] 1) Take out the grown isolated large single-crystal graphene sample, and bake it on a hot table at 150°C for 3-5 minutes to develop the graphene and visualize its position.

[0082] The graphene on the side of the copper foil that does not need to be transferred is removed by bombardment through an air plasma cleaning machine. The air flow is 15 sccm, the power is 90W, and the time is 3 minutes.

[0083] The graphene on the side to be transferred is facing upwards, and the target transmission substrate is facing down, and placed directly above the graphene sample to be transferred. Since the transmission substrate target is a disc with a diameter of 3mm, drop 5-10 microliters of chromatographic purity Propanol, to make isopropanol volatilize naturally, and then heat to 60°C for 10 minutes to ensure the close contact between the substrate an...

Embodiment 2

[0109] Example 2: An aqueous solution of ammonium persulfate encapsulated with high-quality graphene large single-crystal support film with high efficiency

[0110] According to embodiment 1 step 1) the graphene large single crystal thin film sample that has grown is transferred to transmission electron microscope substrate by growth substrate; Step 2)-5) is the same as embodiment 1, only embodiment 1 step 2) is used 20 microliters of the aqueous solution of gold nanoparticles was replaced by 5-8 microliters of ammonium persulfate aqueous solution; the ethanol used in Step 5) of Example 1 was replaced with isopropanol.

[0111] Figure 7 It shows that the metal ribs of the two graphene large single crystal support film grids can be completely stacked after the fixed-point liquid seal, which ensures the maximum area of ​​the liquid-sealed sample. It can be seen that since the light absorption rate of single-layer graphene is only 2.3%, the graphene liquid-sealed area can still...

Embodiment 3

[0116] Embodiment 3: High-efficiency encapsulation of potassium iodide-based lead ammonium (CH 3 NH 3 PB 3 ) butyrolactone solution

[0117] According to embodiment 1 step 1) the graphene large single crystal thin film sample that has grown is transferred to the transmission substrate (that is, the commercial transmission electron microscope microgrid net) from the growth substrate; steps 2)-5) are the same as embodiment 1, only The 1-20 μl aqueous solution of gold nanoparticles used in step 2) of Example 1 was replaced by the butyrolactone solution of lead ammonium iodide; the ethanol used in step 5) of Example 1 was replaced by isopropanol.

[0118] Figure 7 It shows that the metal ribs of the two graphene large single crystal support film grids can be completely stacked after the fixed-point liquid seal, which ensures the maximum area of ​​the liquid-sealed sample. It can be seen that since the light absorption rate of single-layer graphene is only 2.3%, the graphene l...

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Abstract

The invention discloses a method used for realizing high-efficiency liquid packaging using graphene monocrystal support membrane grid. The method comprises following steps: two slices of graphene grow on different growth substrates are transferred onto a transmission substrate, liquid to be packaged is dropped onto the surface of one of the two graphene slices, and the graphene slice is coated with the other graphene slice so as to realize packaging, and obtain a large amount of liquid bubbles for in-situ characterization under a transmission electron microscope. The process is simple; repeatability is high; controllability is high; compatibility is high; thousands of liquid cells packaged with graphene on a sample with a size of several millimeters are prepared in a short time for in-situ characterization under a transmission electron microscope, so that the possibility of study of reaction mechanism on atomic scale is increased greatly.

Description

technical field [0001] The invention belongs to the field of semiconductors, and relates to a method for realizing high-efficiency liquid encapsulation by using a graphene single-crystal support film carrier network. Background technique [0002] Graphene is a carbon atom by sp 2 The single-layer or few-layer two-dimensional crystal material formed by hybridization has excellent electrical, optical and mechanical properties. At the same time, the efficient and relatively low-cost chemical vapor deposition method provides a guarantee for the batch preparation and application of high-quality graphene films. In addition to being used in conventional fields such as transparent conductive films, photodetectors, and biosensors, graphene also has great potential in the field of transmission electron microscopy characterization. The ultra-high electrical conductivity and thermal conductivity can effectively reduce the loss of electron irradiation. The regular structure of the sing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28G01N1/36H01J37/20
CPCG01N1/2806G01N1/2853G01N1/36H01J37/20
Inventor 彭海琳刘忠范张金灿林立谈振军
Owner PEKING UNIV
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