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Liquid phase synthesis method of ultra-thin molybdenum diselenide nanosheet

A liquid-phase synthesis technology of molybdenum diselenide, which is applied in the direction of binary selenium/tellurium compounds, nanotechnology, metal selenide/telluride, etc., can solve the problems of strict preparation conditions, harsh synthesis conditions, and expensive equipment, and achieve Uniform and flat shape, simple method and short preparation period

Inactive Publication Date: 2019-04-16
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthesis conditions by stripping or vapor deposition are generally harsh, or the process is complicated, the preparation conditions are strict, or the equipment is expensive, which limits its practical application.

Method used

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  • Liquid phase synthesis method of ultra-thin molybdenum diselenide nanosheet
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  • Liquid phase synthesis method of ultra-thin molybdenum diselenide nanosheet

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preparation example Construction

[0024] The invention provides a liquid-phase synthesis method of ultra-thin molybdenum diselenide nanosheets, which is characterized in that it comprises the following steps:

[0025] Mixing molybdenum source, selenium source and organic amine, removing impurities to obtain a mixed solution;

[0026] Reacting the mixed solution at 240-300°C for 20-60 minutes to obtain ultra-thin molybdenum diselenide nanosheets;

[0027] The molybdenum source is selected from one or more of ammonium molybdate, sodium molybdate, ammonium phosphomolybdate, molybdenum trioxide, molybdenum acetylacetonate and molybdenum acetate;

[0028] The selenium source is selected from one or more of selenium powder, selenomethionine and dibenzyl diselenide.

[0029] The method provided by the invention adopts common precursors as raw materials, and prepares large-area, ultra-thin molybdenum diselenide nanosheets with relatively uniform and smooth appearance through solution phase synthesis, and the operatio...

Embodiment 1

[0040] Weigh 0.0469g of ammonium phosphomolybdate and 0.034g of dibenzyl diselenide into a 50mL three-necked flask, then add 10mL of oleylamine, and obtain a reaction medium by ultrasonication at room temperature, and introduce argon gas into the reaction system. The reactant was heated to 150°C under low temperature, and kept for 30 minutes to remove some low-boiling impurities, then raised to 240°C, and kept for 30 minutes to complete the reaction. After the reaction, it was naturally cooled to room temperature, and the obtained product was washed several times with n-hexane and acetone, and dispersed in toluene for later use.

[0041] figure 1 It is the X-ray diffraction spectrogram of the molybdenum diselenide nanosheet obtained in Example 1 of the present invention;

[0042] figure 2 It is a transmission electron microscope photo of molybdenum diselenide nanosheets obtained in Example 1 of the present invention;

[0043] image 3 It is an atomic force microscope phot...

Embodiment 2

[0050] Weigh 0.0469g of ammonium phosphomolybdate and 0.051g of dibenzyl diselenide into a 50mL three-necked flask, then add 10mL of oleylamine, and obtain a reaction medium by ultrasonication at room temperature, and feed argon into the reaction system, The reactant was heated to 150°C under low temperature, and kept for 30 minutes to remove some low-boiling impurities, then raised to 260°C, and kept for 30 minutes to complete the reaction. After the reaction, it was naturally cooled to room temperature, and the obtained product was washed several times with n-hexane and acetone, and dispersed in toluene for later use.

[0051] The quality of the product synthesized according to the ratio of Example 2 is 27 mg, the theoretical synthesis product quality is 38 mg, and the yield is 71%.

[0052]As can be seen from the above examples, the present invention provides a liquid-phase synthesis method for ultra-thin molybdenum diselenide nanosheets, comprising the following steps: mix...

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Abstract

The invention provides a liquid phase synthesis method of an ultra-thin molybdenum diselenide nanosheet, which comprises the following steps of: mixing a molybdenum source, a selenium source and organic amine, and removing impurities to obtain a mixed solution; reacting the mixed solution at 240-300 DEG C for 20-60min to obtain an ultra-thin molybdenum diselenide nanosheet; wherein the molybdenumsource is selected from one or more of ammonium molybdate, sodium molybdate, ammonium phosphomolybdate, molybdenum trioxide, oxymolybdenum acetylacetonate and molybdenum acetate; the selenium source is selected from one or more of selenium powder, selenium methionine and dibenzyl diselenium. According to the invention, a precursor source (a molybdenum source and a selenium source) of a specific kind and an organic amine solvent are selected to promote spreading to form an ultra-thin molybdenum diselenide nanosheet with a large area and an uniform and smooth appearance; the raw materials are common raw materials, the conditions are mild, and the method is simple; the method has short preparation period and high yield. The nanosheet has a single-layer or several-layer morphology. That the molybdenum diselenide is a coexistent phase of 1T phase and 2H phase, which can be seen from a photoelectron spectrogram and a high-angle annular dark field image and is beneficial to the improvement ofthe conductivity.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer materials, in particular to a liquid-phase synthesis method of ultrathin molybdenum diselenide nanosheets. Background technique [0002] Molybdenum diselenide (MoSe 2 ) has a graphite-like crystal structure, and six-coordinated molybdenum atoms form a "sandwich" structure between two layers of selenium atoms. This structure is connected by van der Waals force in space, and different stacking methods form different structures. The quantum size effect and the exposure of catalytic active sites make it a good application prospect in photocatalysis, electrocatalysis, energy storage, etc. [0003] Most of the reports on the preparation of large-area single-layer and several-layer molybdenum diselenide are through mechanical exfoliation, liquid phase exfoliation or chemical vapor deposition, but there is no report on the wet synthesis of large-area single-layer and multi-layer. The synthes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y40/00
CPCB82Y40/00C01B19/007C01P2004/24C01P2006/40
Inventor 杨晴周慧楠
Owner UNIV OF SCI & TECH OF CHINA
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