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Preparation method of two-dimensional laminated plate-shaped transition metal sulfide material

A technology of transition metals and two-dimensional materials, applied in chemical instruments and methods, molybdenum sulfide, aluminum compounds, etc., can solve the problems of high pollution, high cost, and difficulty in the preparation of two-dimensional layered molybdenum disulfide materials, and achieve the goal of preparing The effect of simplicity, uniform chemical composition, and diversified product forms

Active Publication Date: 2021-12-17
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a two-dimensional laminated molybdenum disulfide material for the problems of difficult preparation, high cost and high pollution. Preparation method of metal sulfide material, the method is simple, efficient and easy to scale up

Method used

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  • Preparation method of two-dimensional laminated plate-shaped transition metal sulfide material
  • Preparation method of two-dimensional laminated plate-shaped transition metal sulfide material
  • Preparation method of two-dimensional laminated plate-shaped transition metal sulfide material

Examples

Experimental program
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Effect test

Embodiment 1

[0062] Weigh 8 grams of magnesium chloride hexahydrate and 4.8 grams of aluminum chloride hexahydrate, dissolve them in 100 mL of deionized water, and prepare a mixed salt solution, add coprecipitant dilute ammonia solution under vigorous stirring, and adjust the pH of the solution to 10 at the end point. Under stirring, react for 24 hours to obtain a dispersion of magnesium aluminum hydrotalcite.

[0063] Add 2.5 grams of ammonium paramolybdate and 2.5 grams of thiourea to the above dispersion of magnesium aluminum hydrotalcite, mix thoroughly to obtain a composite precursor mixture, then transfer the mixture to a solvent heat kettle, and react at 200°C for 24 hours , cooled naturally to room temperature, the precipitate was separated, washed, and vacuum-dried at 60°C to obtain a composite product of molybdenum disulfide loaded on the surface of the magnesium aluminum hydrotalcite laminate.

[0064] Etching the obtained composite product with molybdenum disulfide on the surfa...

Embodiment 2

[0067] Weigh 6.1 grams of magnesium chloride hexahydrate and 3.6 grams of aluminum chloride hexahydrate, dissolve them in 200 milliliters of deionized water, and prepare a mixed salt solution, and take another 3.6 grams of sodium hydroxide and dissolve them in 200 milliliters of deionized water, and mix them at room temperature The salt solution and the alkali solution are mixed and added to a rotating liquid film reactor to form nucleation, and the mixed solution is crystallized at 100°C for 12 hours under the protection of nitrogen, and the product is centrifuged to neutrality to obtain magnesium aluminum hydrotalcite powder.

[0068] Place the magnesium aluminum hydrotalcite in the quartz boat and put it in the center of the tube furnace, take 5 grams of ammonium molybdate tetrahydrate solid and place it in the quartz boat next to the hydrotalcite quartz boat, take 5 grams of sulfur powder and place it in the tube furnace One end of the air inlet; filled with argon after vac...

Embodiment 3

[0073] Weigh 2.97 g of zinc nitrate hexahydrate, 0.75 g of aluminum chloride hexahydrate, and 1.4 g of hexamethylenetetramine, dissolve in 70 mL of deionized water, stir with a magnetic stirrer until uniformly mixed, and transfer the mixture to a solvent heating kettle , reacted at 120°C for 12 hours, cooled naturally to room temperature, separated, filtered and washed the obtained white precipitate, and then dried in an oven at 80°C to obtain zinc-aluminum hydrotalcite powder.

[0074] The zinc-aluminum double metal hydroxide solid obtained above and 3 grams of ammonium thiomolybdate solid were ball milled at 800rpm for 1 hour, placed in a quartz boat, put into a tubular heating furnace, and heated to 600°C for 3 hours in a nitrogen protective atmosphere , to obtain a composite product with molybdenum disulfide loaded on the surface of the composite zinc-aluminum compound laminate.

[0075] The obtained composite zinc-aluminum compound laminate surface loaded with molybdenum di...

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Abstract

The invention provides a preparation method of a two-dimensional laminate-shaped transition metal sulfide material. The preparation method comprises the following steps: A) preparing a main body laminate composed of divalent and trivalent cations and an anion intercalation hydrotalcite material; B) compounding or separately placing the molybdenum-containing and sulfur-containing precursors and the hydrotalcite material; C) carrying out heat treatment on the system obtained in the step B to obtain a composite product loaded with molybdenum disulfide on the surface; and D) carrying out etching treatment on the obtained composite product, and removing the hydrotalcite converter substrate to obtain the laminated molybdenum disulfide material. Growth regulation and control of the two-dimensional layered molybdenum disulfide nano material are realized through interaction of the layered hydrotalcite material and sulfur-containing and molybdenum-containing compounds, and two-dimensional laminated molybdenum disulfide is obtained. The two-dimensional laminated molybdenum disulfide has the advantages that the size can be adjusted from nanoscale to micron, the dispersity is good, the specific surface area is high, active sites are fully exposed, and the like. The method is wide in raw material source, simple and environment-friendly in preparation and easy to realize large-scale production.

Description

technical field [0001] The invention relates to the field of preparation of two-dimensional materials, in particular to a preparation method of a two-dimensional layered transition metal sulfide material. Background technique [0002] Graphene, a two-dimensional layered material, has attracted extensive attention due to its excellent electrical, optical, mechanical, and electrochemical properties, but graphene in the intrinsic state does not have an energy band gap, which limits its application. Therefore, it has similar Graphene, a layered semiconductor material, has also received increasing attention. As a typical two-dimensional layered transition metal sulfide, molybdenum disulfide has been widely used in the fields of sensors, catalysis, lithium-ion batteries, solar cells, optoelectronic devices, and high-performance composite materials due to its excellent physical and chemical properties. research and application. In addition, compared with layered graphene, molybde...

Claims

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Application Information

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IPC IPC(8): C01G39/06C01F7/00C01G9/00C25B11/075C25B1/04
CPCC01G39/06C01G9/006C25B11/075C25B1/04C01P2002/20C01P2002/22Y02E60/36
Inventor 范同祥
Owner SHANGHAI JIAO TONG UNIV
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