A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell microsphere

A technology of molybdenum disulfide and core-shell microspheres, which can be used in the preparation of microspheres, chemical instruments and methods, microcapsule preparations, etc., can solve the problems of hazards to workers and the environment, complex processes, and difficulties.

Active Publication Date: 2021-06-08
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Zhang et al. prepared MoS by facile chemical vapor deposition (CVD) 2 Deposited on the surface of three-dimensional graphene, thus effectively avoiding the MoS 2 Layer stacking, the prepared composite three-dimensional material exhibits excellent electrochemical performance, and the prepared lithium-ion battery electrode has a high capacity and outstanding cycle stability (small 2013, 9, No. 20,3433–3438), but this method has high requirements for CVD technology, and the process is complex and difficult
Afterwards, Chang's group proposed a hollow MoS 2 The preparation method of nanocages, ammonium tetrathiomolybdate is reduced under the strong reducibility of its hydrazine to generate ammonia gas, and with its assistance, the hollow MoS 2 Nanocages can be formed (J. Mater. Chem. A, 2016, 4, 51–58), however, this method requires the help of the strong reduction of hydrazine, and the large amount of ammonia generated during the preparation process is harmful to the staff and the environment. harmful

Method used

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  • A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell microsphere
  • A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell microsphere
  • A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell microsphere

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Embodiment 1

[0026] A preparation method of molybdenum oxide / molybdenum disulfide core-shell microspheres, comprising the following steps:

[0027] (1) Put the sodium molybdate powder in a tube furnace, and perform high-temperature oxidation and calcination in the air atmosphere for 2 hours to obtain molybdenum oxide particles. The heating rate during the high-temperature calcination process is 10°C / min, and the calcination temperature is 400°C;

[0028] (2) Add urea and tetrathioacetamide to ethanol at a mass ratio of 1:0.3, stir for 20 mins until clarification, then add the molybdenum oxide particles obtained in step (1), stir evenly with ultrasonic, then transfer to hydrothermal reaction In the kettle, hydrothermal synthesis was carried out at 180°C for 24h;

[0029] (3) The reaction product was centrifuged, washed three times with ethanol and deionized water, and vacuum-dried at 60°C for 12 hours to obtain molybdenum oxide / molybdenum disulfide core-shell microspheres.

[0030] figure...

Embodiment 2

[0032] A preparation method of molybdenum oxide / molybdenum disulfide core-shell microspheres, comprising the following steps:

[0033] (1) Put the ammonium tetrathiomolybdate powder in a tube furnace, and perform high-temperature oxidation and calcination in the air atmosphere for 2 hours to obtain molybdenum oxide particles. The heating rate of the high-temperature calcination process is 2°C / min, and the calcination temperature is 300°C ;

[0034] (2) Add urea and tetrathioacetamide to ethanol at a mass ratio of 1:0.4, stir for 30 mins until clarified, then add the molybdenum oxide particles obtained in step (1), stir evenly with ultrasonic, then transfer to hydrothermal reaction In the kettle, hydrothermal synthesis was carried out at 180°C for 24h;

[0035] (3) The reaction product was centrifuged, washed three times with ethanol and deionized water, and vacuum-dried at 60°C for 12 hours to obtain molybdenum oxide / molybdenum disulfide core-shell microspheres.

[0036] f...

Embodiment 3

[0038] A preparation method of molybdenum oxide / molybdenum disulfide core-shell microspheres, comprising the following steps:

[0039] (1) Put the ammonium tetrathiomolybdate powder in a tube furnace, and perform high-temperature oxidation and calcination in the air atmosphere for 2 hours to obtain molybdenum oxide particles. The heating rate during the high-temperature calcination process is 10°C / min, and the calcination temperature is 400°C ;

[0040] (2) Add urea and tetrathioacetamide to ethanol at a mass ratio of 1:0.3, stir for 30 mins until clarification, then add the molybdenum oxide particles obtained in step (1), stir evenly with ultrasonic, then transfer to hydrothermal reaction In the kettle, hydrothermal synthesis was carried out at 180°C for 36h;

[0041] (3) The reaction product was centrifuged, washed three times with ethanol and deionized water, and vacuum-dried at 60°C for 12 hours to obtain molybdenum oxide / molybdenum disulfide core-shell microspheres.

[...

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Abstract

The invention relates to a preparation method of molybdenum oxide / molybdenum disulfide core-shell microspheres, belonging to the technical field of nanocomposite materials. The preparation method of the present invention includes the following steps: (1) placing the molybdenum source in a tube furnace, and performing high-temperature oxidation and calcination in an air atmosphere to obtain molybdenum oxide particles; (2) adding urea and sulfur source to ethanol, stirring until Clarify, then add molybdenum oxide particles, ultrasonically stir evenly, and then transfer to a hydrothermal reaction kettle; (3) centrifuge the product obtained from the reaction, wash and dry in vacuum to obtain molybdenum oxide / molybdenum disulfide core-shell microspheres. The synthesis route of the preparation method of the present invention is simple, easy to operate, and does not need to use additional sacrificial templates and catalysts. At the same time, the prepared microspheres are regular in shape and uniform in size, dispersed independently without agglomeration, and can be widely used in catalysis, batteries, capacitors, and lubrication. and other fields.

Description

technical field [0001] The invention belongs to the field of nanocomposite functional materials, and in particular relates to a preparation method of molybdenum oxide / molybdenum disulfide core-shell microspheres. Background technique [0002] As a remarkable two-dimensional nanomaterial, molybdenum disulfide (MoS 2 ) have been widely used in batteries, photoelectricity, catalysis and other fields. Theoretical studies and experimental results suggest that single-layer or few-layer MoS 2 than ordinary MoS 2 blocks exhibit higher reactivity due to the majority of active sites on MoS 2 , whose base behaves inertly. The two-dimensional layered MoS 2 tends to form a closed structure, and the layers tend to be stacked, which leads to the reduction of exposed edge active sites, making MoS 2 The reactivity is severely reduced. MoS 2 The reactivity of MoS strongly depends on its structure, shape and size, and MoS with controllable shape, structure and size 2 Nanomaterials hav...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02B01J27/051
Inventor 魏取福侯雪斌蔡以兵黄锋林
Owner JIANGNAN UNIV
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