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Organic amine oriented hydrothermal method for preparation of molybdenum disulfide with multiple morphologies

A technology of molybdenum disulfide and organic amines, which is applied in the field of organic amine-directed hydrothermal preparation of molybdenum disulfide with various morphologies, can solve the problems of single morphology of MoS2, product application limitations, poor adjustability, etc., and achieve rich variety, The effect of short charge transport distance and easy operation

Active Publication Date: 2018-05-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The MoS prepared in the above example 2 Most of the morphology is relatively simple, the adjustability is poor, and the application of the obtained products is limited to a certain extent

Method used

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  • Organic amine oriented hydrothermal method for preparation of molybdenum disulfide with multiple morphologies
  • Organic amine oriented hydrothermal method for preparation of molybdenum disulfide with multiple morphologies
  • Organic amine oriented hydrothermal method for preparation of molybdenum disulfide with multiple morphologies

Examples

Experimental program
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Effect test

Embodiment 1

[0024] 3mmol of sodium molybdate Na 2 MoO 4 Dissolve in 30ml of deionized water to form a 0.1M solution, add 12mmol of thiourea according to the S / Mo ratio of 4:1, and stir evenly. Then add 18mmol of ethylenediamine (the molar ratio of ethylenediamine to the molybdenum source is 6), and after fully stirring, the solution is transferred to a 100ml hydrothermal kettle, reacted at 160°C for 12 hours, and naturally cooled to room temperature. Suction filtration, the precipitate was washed with deionized water and absolute ethanol, and dried under vacuum at 70°C overnight to collect MoS 2 sample. The samples were characterized by SEM, and the SEM results showed that the product was a nanoflower-like structure ( figure 1 ).

Embodiment 2

[0026] 4.5 mmol of ammonium molybdate (NH 4 ) 6 Mo 7 o 24 Dissolve in 30ml of deionized water to form a 0.15M solution, add 13.5mmol of L-cysteine ​​according to the S / Mo ratio of 3:1, and stir evenly. Then add 22.5mmol of triethylenetetramine (the molar ratio of triethylenetetramine to molybdenum source is 5), after fully stirring, the solution is transferred to a 100ml hydrothermal kettle, reacted at 180°C for 24 hours, and cooled naturally to room temperature, filtered with suction, washed the precipitate with deionized water and absolute ethanol, dried under vacuum at 70°C overnight, and collected MoS 2 sample.

Embodiment 3

[0028] 6mmol of sodium molybdate Na 2 MoO 4 Dissolve in 30ml of deionized water to form a 0.2M solution, add 12mmol of glutathione according to the S / Mo ratio of 2:1, and stir evenly. Then add the diethylenetriamine of 24mmol (diethylenetriamine and molybdenum source's substance ratio are 4), after fully stirring, this solution is transferred in the 100ml hydrothermal kettle, reacted 36 hours at 200 ℃, naturally cooled to At 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 2sample. The sample was characterized by SEM, and the result showed that the obtained product was a microspherical structure ( figure 2 ).

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Abstract

The invention discloses an organic amine oriented hydrothermal method for preparation of molybdenum disulfide with multiple morphologies. The method includes the steps of: dissolving a certain amountof a molybdenum source, a sulfur source and organic amine in deionized water to form a solution, controlling the concentration of the molybdenum source at 0.1-0.3M, the S / Mo atom ratio of the raw materials at 2:1-4:1, and the ratio of organic amine to the molybdenum source at 2-6; placing the prepared solution in an airtight hydrothermal reaction kettle for reaction for 12-72h, and controlling thereaction temperature at 160-240DEG C; and at the end of reaction, conducting cooling, pumping filtration, washing and drying, thus obtaining MoS2 products of multiple morphologies. The synthesis method provided by the invention has the advantages of mild conditions, simple operation and high controllability, and the prepared products have flower shape, globularity, cylindrical shape and other geometric shapes.

Description

technical field [0001] The invention belongs to the field of inorganic material synthesis, and in particular relates to a method for preparing molybdenum disulfide with various shapes by hydrothermal method guided by organic amines. 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. In addition, molybdenum disulfide is a compound with antimagnetic and semiconducting properties, which has good op...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B82Y40/00
CPCC01G39/06C01P2004/03C01P2004/30C01P2004/32
Inventor 田志坚李佳鹤王冬娥李敏姜玉霞马怀军潘振栋
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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