Synthetic method of single-layer porous molybdenum disulfide

A technology of molybdenum disulfide and synthesis method, which is applied in coating, gaseous chemical plating, metal material coating process, etc., and can solve the problems that molybdenum disulfide is difficult, time-consuming, and prone to aggregation

Inactive Publication Date: 2018-09-28
KUNMING UNIV OF SCI & TECH
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Problems solved by technology

For example, among the above-mentioned methods, the lithium ion intercalation method is a relatively high-efficiency method, but this preparation method is time-consuming, the preparation conditions are relatively harsh, and aggregation is extremely easy to occur. The main disadvantage of intercalation
The hydrothermal method can realize the preparation of molybdenum disulfide nano-films with various morphologies by changing the experimental conditions. However, it is difficult to prepare molybdenum disulfide with uniform layers, which is also a common disadvantage of these methods.
The molybdenum disulfide that has been prepared presents a variety of shapes, such as nano-flower shape, pyramid shape and single-layer single-crystal film, but the single-layer porous shape has not yet been prepared.

Method used

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  • Synthetic method of single-layer porous molybdenum disulfide
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  • Synthetic method of single-layer porous molybdenum disulfide

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Embodiment 1

[0021] Embodiment 1, a kind of synthetic method of monolayer porous molybdenum disulfide, carries out following steps successively:

[0022] (1) Ultrasonic cleaning of the insulating substrate: ultrasonic in acetone, absolute ethanol and deionized water for 5 minutes;

[0023] (2) Weigh 20mg of MoO 3 Powder as the Mo source, and 450mg of sulfur powder as the S source, were poured into different crucibles;

[0024] (3) Dry the cleaned insulating substrate with nitrogen, and MoO 3 The powder is placed in the same crucible, and then placed in the middle high temperature zone of the single temperature zone CVD furnace, the substrate is on the MoO 3 Downstream, place the crucible containing sulfur powder in the low temperature zone upstream;

[0025] (4) Under high vacuum conditions, in an inert gas atmosphere, heat the high temperature zone of the CVD furnace to 650°C at a heating rate of 10°C / min at 50Pa, and keep it warm for 15 minutes; after the reaction is completed, the li...

Embodiment 2

[0026] Embodiment 2, the substrate and MoO in the step (3) in embodiment 1 3 Put them into two crucibles respectively, and the crucible where the substrate is located is located downstream and next to MoO 3 Powder place crucible is placed, and the heating rate in step (4) is changed into 15 ℃ / min, all the other are equal to example 1.

[0027] The AFM of the molybdenum disulfide that embodiment 1 prepares is as figure 1 Shown: It can be seen from the figure that MoS 2 It is in the form of a porous film. In addition, as a supplement, the structure under the pores is scanned by AFM, showing a smooth substrate; combined with the Raman detection map ( figure 2 ), it can be seen that MoS 2 The wavenumber difference △ between the two characteristic peaks is 19.538cm -1 (It is generally believed that the wave number difference △≤20cm -1 is a single layer), so the prepared MoS 2 single-layer porous structure.

[0028] Comparative example 1, the AFM characterization of the moly...

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Abstract

The invention discloses a synthetic method of single-layer porous molybdenum disulfide. In an inert atmosphere, common sulfur powder and MoO3 are adopted to serve as raw materials, the single-layer porous MoS2 grows by the use of a chemical vapor deposition method in the single-temperature region, and the pore diameter is in a nanometer scale; the temperature in the deposition process is controlled to be 650 DEG C at the room temperature, the temperature rising rate cannot be excessively high, the optimal temperature rising rate is 10 DEG C/min, the deposition time is controlled to range from5 minutes to 15 minutes, and preparation of the single-layer porous MoS2 can be accomplished; and strict control over the single-layer porous MoS2 is achieved through ultrasonic cleaning treatment ofa substrate and optimization of preparation parameters such as the sulfur group elemental powder consumption amount, the growth temperature and the growth time.

Description

technical field [0001] The invention relates to the field of molybdenum disulfide material preparation, in particular to a synthesis method of single-layer porous molybdenum disulfide. technical background [0002] In the structure of each layer of molybdenum disulfide, molybdenum atoms will be surrounded by six sulfur atoms, which will form a triangular prism structure, and many Mo-S facets will be exposed on the periphery. These Mo-S faces are in the crystal. From a scientific analysis, this kind of surface has relatively high energy, relatively high surface activity and instability, and can act as a catalytic active center. Because the hexagonal lattice structure of molybdenum disulfide is formed by octahedron and triangular prism structure, it belongs to a relatively stable crystal structure, and the stability of molybdenum disulfide under high temperature and high pressure makes molybdenum disulfide in It has a very wide range of applications in friction lubrication an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C16/30C23C16/44
CPCC23C16/305C23C16/44
Inventor 程文涛蔡金明
Owner KUNMING UNIV OF SCI & TECH
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