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Method for preparing large-size layered orthorhombic MoS2 nano-film of asymmetric structure under hydrothermal condition

An asymmetric structure, nano-film technology, applied in the preparation of nano-composite materials, micro-field, can solve the problems of difficult to obtain large size, poor repeatability and controllability, and cumbersome process.

Active Publication Date: 2015-10-07
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the yield of micromechanical exfoliation is low and the process is cumbersome, and chemical vapor deposition can obtain high-quality single-layer MoS 2 , but at present, its repeatability and controllability are poor, and it is difficult to obtain large-scale continuous films, and the obtained nano-films are mainly a single lateral stacking or vertical stacking layered structure
Hydrothermal method is a simple method to prepare 2D MoS 2 However, it is difficult to prepare two-dimensional MoS with large size, especially crystal element size and orthogonal orientation, by traditional hydrothermal method. 2 nano film

Method used

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  • Method for preparing large-size layered orthorhombic MoS2 nano-film of asymmetric structure under hydrothermal condition
  • Method for preparing large-size layered orthorhombic MoS2 nano-film of asymmetric structure under hydrothermal condition
  • Method for preparing large-size layered orthorhombic MoS2 nano-film of asymmetric structure under hydrothermal condition

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Experimental program
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Effect test

Embodiment 1

[0034] Weigh a certain amount of molybdic acid, dissolve it with ammonia water to obtain ammonium molybdate, evaporate to dryness in a water bath at 50°C to remove excess ammonia, and then dissolve it with a small amount of deionized water to a concentration of 0.01M. A certain amount of thiourea was weighed and dissolved in NMP as an organic solvent with a concentration of 0.03M. Then mix the aqueous solution of ammonium molybdate and the NMP solution of thiourea at a ratio of 1:20, transfer it into a 100mL polytetrafluoroethylene reactor, and react at 180°C for 24h. once, and then dried under vacuum at 60°C to obtain MoS 2 Powder. The obtained orthogonal asymmetric structure MoS2 nano film is micron size.

Embodiment 2

[0036] Weigh a certain amount of molybdic acid, dissolve it with ammonia water to obtain ammonium molybdate, evaporate to dryness in a water bath at 50°C to remove excess ammonia, and then dissolve it with a small amount of deionized water to a concentration of 0.01M. Weigh a certain amount of thiourea, and dissolve it with organic solvent NMP to a concentration of 0.06M. Then mix the aqueous solution of ammonium molybdate and the NMP solution of thiourea at a ratio of 1:20, transfer it into a 100mL polytetrafluoroethylene reaction kettle, and react at 180°C for 24h. ethanol once, and then vacuum dried at 60°C to obtain MoS 2 Powder. In order to improve the crystallinity, the samples were annealed at 800°C for 2h under Ar atmosphere.

Embodiment 3

[0038] Weigh a certain amount of molybdic acid, dissolve it with ammonia water to obtain ammonium molybdate, evaporate to dryness in a water bath at 50°C to remove excess ammonia, and then dissolve it with a small amount of deionized water to a concentration of 0.01M. A certain amount of thiourea was weighed and dissolved in NMP as an organic solvent with a concentration of 0.03M. Then mix the aqueous solution of ammonium molybdate and the NMP solution of thiourea at a ratio of 1:20, transfer it into a 100mL polytetrafluoroethylene reactor, and put the cleaned silicon substrate into the reactor at an inclination angle of ~45° (The size is just enough to make it stuck in the kettle, so as to ensure that the substrate does not move during the reaction process), react at 200 ° C for 24 hours, after the reaction, take out the Si sheet, and you can get a wafer-sized orthogonal asymmetric structure two-dimensional layered MoS 2 Nanofilm (see image 3 ).

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Abstract

The invention discloses a method for preparing a two-dimensional layered MoS2 nano-film of an asymmetric orthorhombic structure under a hydrothermal condition, and belongs to the field of novel micro / nano-material preparation. Ammonium molybdate, thiourea, N-methylpyrrolidone and water are mixed in a certain proportion, and the micron-dimension or even wafer-size MoS2 nano-film of the asymmetric structure is formed under the hydrothermal condition. The nano-film is formed by laterally-stacked nano-layers and vertically-arranged nano-sheets in an orthorhombic mode. The method is simple, and an important preparation method is provided for developing low-cost and high-effect molybdenum disulfide photoelectric devices.

Description

technical field [0001] The invention belongs to the field of preparation of micro-nano composite materials, in particular to a two-dimensional layered molybdenum sulfide (MoS) with large size and orthogonal asymmetric structure. 2 ) Preparation method of nano film. technical background [0002] As a typical transition metal sulfide semiconductor material, two-dimensional MoS 2 It has excellent electrical, thermal, mechanical and optical properties. Existing studies have shown that MoS 2 It has special advantages and great potential in the fields of catalysis, batteries, hydrogen storage, light-emitting devices, photodetection, laser mode-locking, etc. [1-6] . While two-dimensional MoS 2 Compared with bulk materials, its bandgap is adjustable, and it can be adjusted between 1.3 and 1.9eV with different layers. At the same time, its electronic and photonic properties have significant changes compared with bulk materials. Such as bulk material MoS 2 It is an indirect ban...

Claims

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Application Information

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IPC IPC(8): C03C17/22C04B41/50
Inventor 张晓艳张龙王俊
Owner SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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