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
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[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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