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Method for preparing multilayer molybdenum disulfide in one step

A technology of molybdenum disulfide and insulating substrate, applied in coating, gaseous chemical plating, metal material coating process, etc., can solve the problems of difficult, time-consuming and harsh preparation conditions of molybdenum disulfide

Inactive Publication Date: 2018-10-19
KUNMING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this preparation method is time-consuming, the preparation conditions are relatively harsh, and aggregation is extremely easy to occur, which is the main disadvantage of the lithium ion intercalation method.
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 application of CVD method is relatively common, but no one has used CVD in a single temperature zone to prepare MoS with uniform layer number controllable 2 Come

Method used

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  • Method for preparing multilayer molybdenum disulfide in one step
  • Method for preparing multilayer molybdenum disulfide in one step
  • Method for preparing multilayer molybdenum disulfide in one step

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1, a kind of method for preparing multilayer molybdenum disulfide in one step, 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 500mg 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 750°C at a heating rate of 15°C / min at 50Pa, and keep it warm for 25min; after the reaction is completed, the ...

Embodiment 2

[0026] Embodiment 2, the MoO of step (2) in embodiment 1 3 Powder weight is changed into 15mg, and sulfur powder weight is changed into 400mg, and the soaking time in step (4) is changed into 15min, and all the other are equal to example 1.

[0027] The AFM of the molybdenum disulfide prepared in embodiment 1 is as figure 1 Shown: It can be seen from the figure that there are at least 7 layers of structure, combined with the Raman detection map ( figure 2 ), it can be seen that MoS 2 The wavenumber difference △ between the two characteristic peaks is 26.652cm -1 (It is generally believed that the wave number difference △≤20cm -1 is a single layer), so the prepared MoS 2 For multi-layer structure.

[0028] Comparative example 1, the AFM characterization of the molybdenum disulfide that embodiment 2 prepares is as image 3 As shown, it can be seen from the figure that there are at least 3 layers of structure, combined with Raman detection such as Figure 4 As shown, the ...

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Abstract

The invention discloses a method for preparing multilayer molybdenum disulfide in one step. In an inert atmosphere, common sulfur powder and MoO3 are used as raw materials, multilayer MoS2 is grown incontrol by using chemical vapor deposition method in a single temperature zone, and the number of layers is 3 to 7; the temperature during deposition is controlled at 650 DEG C to 750 DEG C and the deposition time is controlled at 5 to 30 minutes to complete the preparation of multilayer MoS2; and strict control of multilayer MoS2 is realized by optimization of the preparation parameters such asultrasonic cleaning treatment of the substrate, amount of sulfur powder, growth temperature and growth time.

Description

technical field [0001] The invention relates to the field of molybdenum disulfide material preparation, in particular to a method for preparing multilayer molybdenum disulfide in one step. technical background [0002] Most of the layered structures are easy to slip off due to the relatively weak van der Waals force between the layers, and molybdenum disulfide is a typical layered structure. When the molybdenum disulfide layer slides between layers, each shed molybdenum disulfide layer makes it have a relatively low coefficient of friction. This feature makes molybdenum disulfide realize its wide application in the field of lubricants. 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...

Claims

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Application Information

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