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Two-dimensional nano-molybdenum disulfide and preparation method thereof

A molybdenum disulfide and two-dimensional nanotechnology are applied in the field of two-dimensional nano-layered structure molybdenum disulfide materials and their preparation fields, and can solve the problems of cumbersome preparation process, shortened preparation cycle, and disadvantageous mass production.

Active Publication Date: 2017-02-08
厦门宇树康信息技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For example, Chinese patent application CN 201210057757.5 discloses a single-layer MoS 2 The preparation method of nanosheet solution, which improves the liquid phase exfoliation, can shorten the preparation cycle, MoS 2 The dispersibility and stability are improved, but its preparation process is cumbersome, which is not conducive to mass production
Chinese patent CN 102398920 B reports a method for preparing two-dimensional nanomolybdenum disulfide by an improved liquid phase exfoliation method, but this method has higher requirements for equipment
[0006] Vapor deposition method can get better quality MoS 2 Nanosheets, but its operation and process are more complicated, and the cost is higher; the electrochemical method is simple and efficient, but it is difficult to prepare large-area MoS 2 Nanosheets; hydrothermal method is cheap but time-consuming and MoS 2 The number of layers of nanosheets is not easy to control
The traditional thermal decomposition method uses ammonium tetrathiomolybdate ((NH 4 ) 2 MoS 4 ) as a raw material mixed with an organic solvent such as dimethylformamide (DMF) into a solution, and coated on sapphire, SiO 2 Or a thin film is formed on the surface of the Si substrate, and MoS is obtained through multi-step pyrolysis treatment 2 Nanosheets, this method prepares two-dimensional nano-MoS with larger size and better quality 2 , but the preparation process is cumbersome, the stability is poor, and it is not easy to realize industrial production

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  • Two-dimensional nano-molybdenum disulfide and preparation method thereof
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  • Two-dimensional nano-molybdenum disulfide and preparation method thereof

Examples

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Effect test

Embodiment 1

[0027] (1) Add 25g of ammonium paramolybdate tetrahydrate (also known as ammonium paramolybdate, ammonium heptamolybdate) into 60ml of concentrated ammonia water, stir until completely dissolved, then add 240ml of ammonium sulfide solution, and then place the mixed solution in a heating furnace Heating at 50~60°C for 20 minutes to form a dark red mother liquor.

[0028] (2) Use a 1000ml beaker to measure 100ml of the mother liquor, add 14g of glycine, wait for the glycine to fully dissolve and then stir for 10 minutes to form a mixed solution. The temperature of the mother liquor is always kept at 60~70°C during the above process.

[0029] (3) Add 24g of ammonium nitrate to the mixed solution containing the mother liquor and glycine, and stir until the ammonium nitrate is completely dissolved. During the above process, keep the temperature of the mixed solution at 60~70°C. After the ammonium nitrate is completely dissolved, raise the heating temperature To 200~230°C, continue ...

Embodiment 2

[0033] (1) Add 25g of ammonium paramolybdate tetrahydrate into 60ml of concentrated ammonia water, stir until completely dissolved, then add 240ml of ammonium sulfide solution, then place the mixed solution in a heating furnace and heat at 50~60°C for 20 minutes to form a deep red color mother liquor.

[0034] (2) Use a 1000ml beaker to measure 100ml of the mother liquor, add 10g of glycine, wait for the glycine to fully dissolve and then stir for 10 minutes to form a mixed solution. The temperature of the mother liquor is always kept at 60~70°C during the above process.

[0035] (3) Add 23g of ammonium nitrate to the above mixed solution containing mother liquor and glycine, and stir until the ammonium nitrate is completely dissolved. During the above process, keep the temperature of the mixed solution at 60~70°C. After the ammonium nitrate is completely dissolved, raise the heating temperature To 200~230°C, continue heating and stirring.

[0036](4) The above solution is co...

Embodiment 3

[0039] (1) Add 25g of ammonium paramolybdate tetrahydrate into 60ml of concentrated ammonia water, stir until completely dissolved, then add 240ml of ammonium sulfide solution, then place the mixed solution in a heating furnace and heat at 50~60°C for 20 minutes to form a deep red color mother liquor.

[0040] (2) Use a 1000ml beaker to measure 100ml of the mother liquor, add 8g of glycine, wait for the glycine to fully dissolve and then stir for 10 minutes to form a mixed solution. The temperature of the mother liquor is always kept at 60~70°C during the above process.

[0041] (3) Add 18g of ammonium nitrate to the above mixed solution containing mother liquor and glycine, and stir until the ammonium nitrate is completely dissolved. During the above process, keep the temperature of the mixed solution at 60~70°C. After the ammonium nitrate is completely dissolved, raise the heating temperature To 200~230°C, continue heating and stirring.

[0042] (4) The above solution is co...

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Abstract

The invention discloses two-dimensional nano-molybdenum disulfide and a preparation method thereof. Ammonium paramolybdate tetrahydrate serving as a molybdenum source is added into stronger ammonia water, an ammonium sulfide solution is used as a sulfur source, and ammonium nitrate and glycine are used as reaction fuel; molybdenum disulfide with a two-dimensional nano laminar structure is prepared by using chalcophile oxygen hydrophobic properties of molybdenum through vulcanization reaction and high-temperature decomposition. The preparation method adopts the following preparation process flow: preparing a mother solution, adding the glycine, adding the ammonium nitrate, performing reactive synthesis, and obtaining the two-dimensional nano-molybdenum disulfide. The particle size of two-dimensional nano-molybdenum disulfide powder prepared by the process is 30 to 100nm; the layer number of most molybdenum disulfide is 2 to 6, and the layer space is 0.60 to 0.69nm. The invention provides a simple and efficient method for preparing two-dimensional nano laminar molybdenum disulfide.

Description

technical field [0001] The invention belongs to the field of synthesis and preparation of two-dimensional nano-layered materials, and particularly provides a molybdenum disulfide material with a two-dimensional nano-layered structure and a preparation method thereof. Background technique [0002] Molybdenum disulfide (MoS 2 ) is a layered material with excellent properties that has emerged in recent years, and it has good application prospects in the fields of electrochemistry, lubricating machinery, catalysis, and intercalation chemistry. When the particle size of molybdenum disulfide reaches the nanoscale, that is, two-dimensional molybdenum disulfide, due to the larger specific surface area of ​​nano-molybdenum disulfide, the reactivity of the particles is high, and its many properties, such as adsorption performance, catalytic performance and electrochemical performance, etc. will be further improved. In addition, because the energy band spacing of nanoscale molybdenum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B82Y40/00
CPCC01G39/06C01P2002/01C01P2002/20C01P2002/72C01P2004/03C01P2004/64
Inventor 古思勇张厚安张勇麻季冬马丽丽廉冀琼陈莹
Owner 厦门宇树康信息技术有限公司
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