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Polyatomic co-doped molybdenum disulfide and preparation method and application thereof

A technology of molybdenum disulfide and atoms, applied in the field of preparation of two-dimensional nanomaterials

Inactive Publication Date: 2020-10-30
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

However, it is necessary to ensure that the original molybdenum disulfide "sandwich" structure (S-Mo-S) is not damaged when multiple elements are doped at the same time, and it is also necessary to avoid agglomeration or formation of new phases between various doping elements. , such a preparation strategy is quite challenging

Method used

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  • Polyatomic co-doped molybdenum disulfide and preparation method and application thereof
  • Polyatomic co-doped molybdenum disulfide and preparation method and application thereof
  • Polyatomic co-doped molybdenum disulfide and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Dissolve 400mg of ammonium molybdate and 359mg of cobalt nitrate in 20mL of water. After ultrasonic dispersion for 1 hour, continue to add 55.5mg of selenium powder. Carbon disulfide was sealed into a 60mL autoclave under the protection of argon.

[0037] 2. Keep the autoclave in (1) at 200°C for 4h.

[0038] 3. the sample obtained in (2) in 6mol L -1 Potassium hydroxide solution for 5h. Then wash with ultrapure water and ethanol and filter with suction.

[0039] 4. Dry the sample obtained in (3) at 80° C. for 12 hours to obtain template-free cobalt-selenium co-doped molybdenum disulfide.

[0040] TEM (see figure 1 a) show that the obtained samples are all flower-like structures, high-resolution electron microscopy (see figure 1b) shows that the obtained sample has a two-dimensional layered structure, and the number of layers is mostly a few layers, and no other clusters or impurity phases appear. X-ray diffraction spectrum (see image 3 ) shows that the obtai...

Embodiment 2

[0042] 1. Put 400mg of ammonium molybdate and 2.5g of silicon dioxide in 20mL of water, ultrasonically disperse for 0.5h, then add 359mg of cobalt nitrate and ultrasonically disperse for 1h, continue to add 55.5mg of selenium powder, after ultrasonically mixing for 1h, stir at 25°C for 12h , dried at 60°C for 12h, and then sealed with 10mL of carbon disulfide in a 60mL autoclave under the protection of argon.

[0043] 2. Keep the autoclave in (1) at 200°C for 4h.

[0044] 3. Treat the sample obtained in (2) with 5% hydrofluoric acid solution for 12 hours. Then wash with ultrapure water and ethanol and filter with suction.

[0045] 4. Dry the sample obtained in (3) at 80° C. for 12 hours to obtain cobalt-selenium co-doped molybdenum disulfide with a template. TEM (see figure 2 a) shows that the obtained samples are all three-dimensional foam-like structures, high-resolution electron microscope (see figure 2 b) It shows that the obtained sample has a two-dimensional layere...

Embodiment 3

[0053] 1. Ultrasonic disperse 400mg ammonium molybdate and 2.5g silicon dioxide in 30mL water for 0.5h, add 159mg cobalt nitrate and 150mg nickel nitrate and ultrasonically disperse for 2h, then stir at 25°C for 12h, dry at 60°C for 12h, and then mix with 10mL of carbon disulfide was sealed into a 60mL autoclave under the protection of argon.

[0054] 2. Keep the autoclave in (1) at 400°C for 4h.

[0055] 3. Treat the sample obtained in (2) with 5% hydrofluoric acid solution for 12 hours. Then wash with ultrapure water and ethanol and filter with suction.

[0056] 4. Dry the sample obtained in (3) at 80° C. for 12 hours to obtain templated cobalt-nickel co-doped molybdenum disulfide.

[0057] The transmission electron microscope showed that the obtained sample had a three-dimensional foam-like structure, and the high-resolution electron microscope showed that the obtained sample had a two-dimensional layered structure, and it was a vertically stacked array structure with abu...

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Abstract

The invention discloses a preparation method of polyatomic co-doped molybdenum disulfide. Specifically, the method comprises the following steps: firstly, uniformly dispersing a plurality of doped atom precursors with a molybdenum source in sequence, then reacting with a sulfur-containing compound at a certain temperature, finally, carrying out solution treatment, and carrying out suction filtration and drying to obtain a target product. The material prepared by the method has a clear structure, a single crystal image and no cluster or non-molybdenum disulfide crystal image formation. The types and the contents of the doped heteroatoms are easy to modulate. The material has excellent activity when being used for electrocatalytic hydrogen evolution reaction. The method is a universal methodfor preparing polyatomic co-doped molybdenum disulfide, and has the characteristics of being simple and easy to operate.

Description

technical field [0001] The invention belongs to the technical field of preparation of two-dimensional nanometer materials, and in particular relates to a polyatomic co-doped molybdenum disulfide and its preparation method and application. Background technique [0002] Two-dimensional molybdenum disulfide has attracted widespread attention due to its unique structure and electronic properties, and has good application prospects in materials science, chemistry, and nanotechnology. Especially in the electrocatalytic hydrogen evolution reaction, because of its large earth reserves, environmental friendliness, and superior performance, it is expected to become a good substitute for platinum-based electrocatalysts. However, the hydrogen evolution activity of molybdenum disulfide mainly comes from its small amount of edge sites, while most of its in-plane sites are relatively inert (B.Hinnemann, J.K. et al. J. Am. Chem. Soc., 127, 5308-5309 (2005)). Based on this understanding,...

Claims

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Application Information

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IPC IPC(8): C01G39/06B01J27/051
CPCB01J27/051C01G39/06C01P2006/40
Inventor 邓德会郑智龙孟祥宇毛军
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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