Method for preparing two-dimensional atomic crystal new material by supercritical fluid

A two-dimensional atomic crystal, supercritical flow technology, applied in the direction of polycrystalline material growth, crystal growth, chemical instruments and methods, etc., can solve the problem that the same quality standard of graphene cannot be reached, large-scale production cannot be promoted, and preparation methods are single, etc. problem, to achieve the effect of mild conditions, controllable number of layers, and simple process

Active Publication Date: 2012-10-17
SHANGHAI JIAO TONG UNIV
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  • Abstract
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Problems solved by technology

Novoselov and Geim, who won the Nobel Prize for the first successful preparation of graphene, can only use micromechanical methods to peel off extremely small and inefficient raw materials of layered materials; as of 2011, only Ireland Jonathan N. Coleman published an article in Science magazine about the use of liquid exfoliation technology to prepare two-dimensional planar atomic crystal thin films. The disadvantages of liquid dissociation are its long production cycle, harsh reaction conditions, and cumbersome and complicated processes.
Worldwide, research on boron nitride thin films is still in its infancy, and its preparation methods are relatively simple. Except for the micromechanical stripping method used by Nobel Prize winners, only chemical synthesis and chemical vapor deposition have been reported. Considering product quality, preparation process, economic cost, etc., it is still unable to meet the same quality standards as graphene, let alone promote large-scale production

Method used

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  • Method for preparing two-dimensional atomic crystal new material by supercritical fluid
  • Method for preparing two-dimensional atomic crystal new material by supercritical fluid
  • Method for preparing two-dimensional atomic crystal new material by supercritical fluid

Examples

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Embodiment 1

[0030] A method for preparing a new two-dimensional atomic crystal material using a supercritical fluid, the method adopts a device such as figure 1 As shown, it includes a carbon dioxide cylinder 1, a cooling device 2, a carbon dioxide pump 3, a pressure controller 4, a high-pressure reaction kettle 5, and a pressure relief sample collection tank 6. When in use, add 50 mg of hexagonal boron nitride powder into the autoclave 5 . The autoclave temperature was set at 45 °C. Carbon dioxide is pumped into the autoclave 5 through the carbon dioxide pump 3, and the pressure in the autoclave is controlled at 15MPa. The material stays in the autoclave 5 for 120 minutes, and the pressure is released at a rate of 0.2 atm / s to collect the product. Through atomic force microscope test and characterization, the large-scale hexagonal boron nitride thin film with tens of microns and less than 10 atomic layers in the product is more than 30%, and its characterization photos are as follows ...

Embodiment 2

[0032] Add 50 mg of hexagonal boron nitride powder into the autoclave 5 . The autoclave temperature was set at 45 °C. Carbon dioxide is pumped into the autoclave 5 through the carbon dioxide pump 3, and the pressure in the autoclave is controlled at 15MPa. The material stays in the high-pressure reactor 5 for 120 minutes, 60W ultrasonic vibration is applied to the supercritical system for 30min, and the pressure is released at a rate of 0.2atm / s. The product is collected and characterized by atomic force microscopy. The hexagonal boron nitride film below the layer is greater than 60%, and there is a monoatomic layer boron nitride film, and the photo of its characterization is as follows figure 2 shown.

Embodiment 3

[0034] Add 50 mg of hexagonal boron nitride powder into the autoclave 5 . The autoclave temperature was set at 45 °C. Carbon dioxide is pumped into the autoclave 5 through the carbon dioxide pump 3, and the pressure in the autoclave is controlled at 15MPa. The material stays in the high-pressure reactor 5 for 120 minutes, 30min 60W ultrasonic oscillation is applied to the supercritical system, and the system is repeatedly pressurized and depressurized 5 times at a depressurization rate of 0.2atm / s. The collected product is characterized by atomic force microscopy. The product Medium and large-scale hexagonal boron nitride films with less than 5 atomic layers in the order of tens of microns are more than 56%, and monoatomic layer boron nitride films show a relatively large proportion, about 14%.

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Abstract

The invention relates to method for preparing a two-dimensional atomic crystal new material by supercritical fluid. The method comprises the steps of: by taking laminated structure materials such as boron nitride (BN), molybdenum disulfide (MoS2), tungsten disulfide (WS2) as raw materials, and taking supercritical fluid (carbon dioxide CO2) as a stripping agent, successfully stripping new two-dimensional atomic crystal material for preparing BN film, MoS2 film, WS2 film and the like, wherein each film exists in a form of a single layer (monoatomic layer) and a few thin layers (a few atomic layers). The two-dimensional atomic crystal film prepared by the method has the same or similar structure with graphene, and has excellent mechanical property and transmittance property. Each film has excellent electrical, magnetic, thermal and optical performance, and has important application prospect in many fields; and by the technology of preparing the two-dimensional atomic crystal film by supercritical fluid in a stripping way, the product film has the advantages of controllable layers, excellent structure, high yield, simple process and low cost.

Description

technical field [0001] The invention belongs to the technical field of preparation of advanced functional materials, and in particular relates to a method for preparing a two-dimensional atomic crystal new material by using a supercritical fluid, including preparing hexagonal boron nitride BN thin film, MoS 2 Film, WS 2 Films and corresponding films of other layered structural materials. Background technique [0002] The discovery of graphene, a single atomic layer material, broke the traditional theoretical estimation that single atomic layer graphite cannot exist stably alone; graphene is more famous for its perfect two-dimensional single atomic layer, unique optical properties, super strong mechanical toughness, excellent The electrical properties have conquered the physicists who pursue perfection; the structural characteristics of the multi-center large π bond make it possible to bond with various groups and functional groups, thus determining its extremely rich chemic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B30/06C30B29/68
Inventor 周城宏赵亚平忻娜王燕王武聪
Owner SHANGHAI JIAO TONG UNIV
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