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Method for complexing hydrothermal synthesis of uniform flower-like MoS2 nanospheres

A hydrothermal synthesis, nanotechnology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of small specific surface, low activity, large, mostly at the micron level, etc., to reduce The effect of agglomeration, high reactivity and many active sites

Inactive Publication Date: 2016-03-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since ionic liquids are generally macromolecules, they form MoS after self-assembly in aqueous solution. 2 The grown template, the prepared product has a larger size, mostly at the micron level, with a smaller specific surface area and lower activity

Method used

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  • Method for complexing hydrothermal synthesis of uniform flower-like MoS2 nanospheres
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  • Method for complexing hydrothermal synthesis of uniform flower-like MoS2 nanospheres

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Experimental program
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Effect test

Embodiment 1

[0026] Dissolve 5mmol of sodium molybdate in 50ml of deionized water to form a 0.1M solution, add 20mmol of potassium sulfide, and stir evenly. Then 12 mmol of oxalic acid was added. After fully stirring, transfer the solution to a 100ml hydrothermal kettle, react at 120°C for 24 hours, naturally cool to room temperature, filter with suction, wash the precipitate with deionized water and absolute ethanol, dry it under vacuum at 70°C overnight, and collect MoS 2 sample. The samples were characterized by SEM, and the SEM results showed that the obtained product was nano-curds with a particle size of about 200nm, and the curds were formed by a large number of lamellar structures with good dispersion.

Embodiment 2

[0028] Dissolve 3.5mmol of sodium molybdate in 50ml of deionized water to form a 0.07M solution, add 12mmol of ammonium sulfide, and stir evenly. Then 8.3 mmol of oxalic acid was added. After fully stirring, transfer the solution to a 100ml hydrothermal kettle, react at 140°C for 36 hours, naturally cool to room temperature, filter with suction, wash the precipitate with deionized water and absolute ethanol, dry it under vacuum at 70°C overnight, and collect MoS 2 sample. The samples were characterized by SEM, and the SEM results showed that the obtained product was nano-curds with a particle size of about 300nm, and the curds were formed by lamellar structures with good dispersion.

Embodiment 3

[0030] Dissolve 2.5mmol of ammonium molybdate in 50ml of deionized water to form a 0.05M solution, add 10mmol of ammonium sulfide, and stir evenly. Then 7.5 mmol of oxalic acid was added. After fully stirring, transfer the solution to a 100ml hydrothermal kettle, react at 160°C for 48 hours, naturally cool to room temperature, filter with suction, wash the precipitate with deionized water and absolute ethanol, dry it under vacuum at 70°C overnight, and collect MoS 2 sample. The samples were characterized by SEM, and the SEM results showed that the obtained product was nano-curds with a particle size of about 200-300nm, and the curds were formed by stacking lamellar structures with good dispersion.

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Abstract

The present invention discloses a method for complexing hydrothermal synthesis of uniform flower-like MoS2 nanospheres. The method comprises: sequentially dissolving a certain amount of a molybdenum source, a sulfur source and a complexing agent in deionized water to form a solution, regulating the molybdenum source concentration to 0.04-0.16 M, regulating a molar ratio of the sulfur source to the molybdenum source to 2:7-4:1, and regulating a molar ratio of the complexing agent to the molybdenum source to 2-6; placing the prepared solution in a closed hydrothermal reaction kettle, controlling the reaction temperature at 120-200 DEG C, and controlling the reaction time at 24-72 h; and after completing the reaction, cooling, carrying out suction filtration, washing, and drying to obtain the flower-like MoS2 nanospheres. According to the present invention, the synthesis method has advantages of mild condition, simple operation, uniform product morphology and particle size, good product dispersion property, and high yield; and the synthesized flower-like MoS2 nanospheres adopted as oil product hydrogenation catalysts, electrode materials, solid lubricants and the like have wide applications.

Description

technical field [0001] The invention belongs to the field of synthesis of inorganic nanomaterials, in particular to a complex hydrothermal synthesis of uniform MoS 2 The nanocurd method. Background technique [0002] MoS 2 It is the main component of molybdenite, and there is a sandwich type layer in its crystal structure: a layer of Mo atoms is sandwiched between two layers of S atoms, forming a "sandwich" sandwich structure. The atoms in the layers are bonded by strong covalent bonds, and the weaker Van der Waals force between the layers makes it easy to peel off between layers, with good anisotropy and low friction coefficient. MoS 2 Each molybdenum atom in the crystal is surrounded by six sulfur atoms, in the shape of a triangular prism, exposing many Mo-S facets, which can be used as catalytic active centers. The nano-intercalation composites formed after inserting other groups between the layers have many excellent physical properties. In addition, molybdenum disu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B82Y30/00B82Y40/00
Inventor 田志坚李佳鹤王冬娥姜玉霞李敏马怀军潘振栋曲炜李鹏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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