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Preparation method for ion liquid assisted hydrothermal synthesis of MoS2 microsphere

An ionic liquid and hydrothermal synthesis technology, applied in the direction of molybdenum sulfide, etc., can solve the problems of thermal synthesis of MoS2 microspheres that have not been reported publicly, and achieve the effects of high yield, good reproducibility, and simple process

Inactive Publication Date: 2007-07-11
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, ionic liquid-assisted hydrothermal synthesis of MoS 2 The literature and patents of microspheres have not yet been published

Method used

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  • Preparation method for ion liquid assisted hydrothermal synthesis of MoS2 microsphere

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Experimental program
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Effect test

Embodiment 1

[0027] Dissolve 3mmol of sodium molybdate in 30ml of deionized water to form a 0.1M solution, add 9mmol of thioacetamide, and stir evenly. Then add 0.5ml of ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF 4 ], after fully stirring, the solution was transferred to a 50ml reaction kettle, hydrothermally reacted at 240°C for 24 hours, then cooled naturally, and the synthesized MoS was collected after being fully washed by centrifugation and deionized water and dried in vacuum. 2 sample. As a comparison, under the same conditions, MoS was synthesized with the same process steps without the addition of ionic liquids 2 sample. The above two samples were characterized by XRD and SEM, and the XRD diffraction patterns of the two were found to be consistent with MoS 2 standard XRD diffraction card, but containing MoS hydrothermally synthesized by ionic liquid (volume ratio of ionic liquid to synthesis solution is 1:60) 2 The sample aggregates in the form of micr...

Embodiment 2

[0029] Dissolve 3mmol of sodium molybdate in 60ml of deionized water to form a 0.05M solution, add 15mmol of thiourea, and stir evenly. Then add 0.2ml of ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF 4 ], after fully stirring, the solution was transferred to a 100ml reaction kettle, and the hydrothermal reaction was carried out at 230 °C for 23 hours, then cooled naturally, and the synthesized MoS was collected after being fully washed by centrifugation and deionized water and dried in vacuum. 2 Sample, SEM characterization of the sample, SEM photos show ionic liquid assisted hydrothermal synthesis (the ratio volume of ionic liquid to synthesis solution is 1:300) of MoS 2 The samples aggregated in the form of microspheres with an average diameter of 1.3 microns (see Figure 2).

Embodiment 3

[0031]Dissolve 3.6mmol of sodium molybdate in 60ml of deionized water to form a 0.06M solution, add 10.8mmol of thioacetamide, and stir evenly. Then add 0.6ml of ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF 4 ], the solution was transferred to a 100ml reactor after being fully charged, and the hydrothermal reaction was carried out at 220°C for 21 hours, and then cooled naturally, and the synthesized MoS was collected after being fully washed with centrifugation and deionized water and dried in vacuum. 2 Sample, SEM characterization of the sample, SEM photos show ionic liquid assisted hydrothermal synthesis (volume ratio of ionic liquid to synthesis solution is 1:100) of MoS 2 The samples aggregated in the form of microspheres with an average diameter of 2.1 microns.

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Abstract

The invention discloses a making method of MoS2 microball synthesized by ionic liquid auxiliary water, which comprises the following steps: dissolving molybdate in the deionized water to form 0.05-0.1m solution; adding thioacetamide or sulfourea as sulfur source with molar rate of thioacetamide or sulfourea and molybdate at 31-51; stirring evenly; adding 1-butyl-3-methyl imidazole tetrafluoride borate as ionic liquid with the bulk rate of ionic liquid and synthetic solution at 1300-1 50; stirring completely; transmitting solution into water heat reacting autoclave to react under 200-240 deg. c for 20-24h; cooling naturally; separating; washing; drying to obtain the product.

Description

technical field [0001] The invention relates to the preparation of inorganic nanomaterials, in particular to an ionic liquid-assisted hydrothermal synthesis of MoS 2 Preparation method of microspheres. Background technique [0002] MoS 2 Belonging to the hexagonal crystal system, it is a typical sandwich layered structure. There are strong covalent bonds in the layers, and weak van der Waals forces between the layers. The layers are easy to peel off. It has good anisotropy and low friction coefficient, and S has strong adhesion to metal, making MoS 2 It can be well attached to the metal surface and always play a lubricating function, especially under the conditions of high temperature and high vacuum, it still has a low friction coefficient, so it is an excellent solid lubricant. In addition, MoS with a layered structure 2 As the host lattice, it can react with different guest atoms or molecules, and the guest atoms or molecules are inserted between the host layers to pr...

Claims

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Application Information

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IPC IPC(8): C01G39/06
Inventor 马琳陈卫祥李辉赵杰
Owner ZHEJIANG UNIV
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