Preparation method of heteroatom doped porous molybdenum disulfide coated graphene

A technology of molybdenum disulfide and graphene, which is applied in the direction of chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., to achieve the effect of facilitating the application of the method, wide application range, and good conductivity

Inactive Publication Date: 2019-11-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But effectively wrapping three-dimensional molybdenum disulfide on foamy graphene is not a small challenge

Method used

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  • Preparation method of heteroatom doped porous molybdenum disulfide coated graphene
  • Preparation method of heteroatom doped porous molybdenum disulfide coated graphene
  • Preparation method of heteroatom doped porous molybdenum disulfide coated graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1. Disperse 400mg of silica spheres in 200mL of ethanol, then reflux with 4mL of (3-aminopropyl)trimethoxysilane at 180°C for 5 hours, then add 0.8% graphene oxide water dispersion 3.7 g, stirred.

[0047] 2. Mix the sample obtained in (1) with 33 mg of ammonium molybdate, and dry at 80° C. for 5 hours.

[0048] 3. The sample obtained in (2) was transferred with 10 mL of carbon disulfide and sealed in a 60 mL autoclave in an argon atmosphere.

[0049] 4. React the autoclave in (3) at 400° C. for 9 hours.

[0050] 5. Treat the sample obtained in (4) with a 5% hydrofluoric acid solution by mass fraction for 8 hours, then wash with water, suction filter, and dry at 80° C. for 8 hours.

[0051] TEM (see figure 1 ) shows that the obtained sample has regular and uniform sponge-like three-dimensional channels, and the molybdenum disulfide single hole is evenly wrapped on the outer wall of the graphene single hole. X-ray diffraction spectrum (see Figure 4 Middle a) shows ...

Embodiment 2

[0053] 1. Disperse 400mg of silica spheres in 200mL of ethanol, then reflux with 4mL of (3-aminopropyl)trimethoxysilane at 180°C for 5 hours, then add 0.8% graphene oxide water dispersion 3.7 g, stirred.

[0054] 2. Mix the sample obtained in (1) with 33 mg of ammonium molybdate and 24 mg of cobalt nitrate, and dry at 80° C. for 5 hours.

[0055] 3. The sample obtained in (2) was transferred with 10 mL of carbon disulfide and sealed in a 60 mL autoclave in an argon atmosphere.

[0056] 4. React the autoclave in (3) at 400° C. for 9 hours.

[0057] 5. Treat the sample obtained in (4) with a 5% hydrofluoric acid solution by mass fraction for 8 hours, then wash with water, suction filter, and dry at 80° C. for 8 hours.

[0058] TEM (see figure 2 a) shows that the obtained sample has regular and uniform three-dimensional pores, and the high-resolution transmission electron microscope picture (see figure 2 b) It shows that the molybdenum disulfide single hole is evenly wrappe...

Embodiment 3

[0060] 1. Disperse 400mg of silica spheres in 200mL of ethanol, then reflux with 4mL of (3-aminopropyl)trimethoxysilane at 180°C for 5 hours, then add 0.8% graphene oxide water dispersion 3.7 g, stirred.

[0061] 2. Mix the sample obtained in (1) with 33 mg of ammonium molybdate and 12 mg of cobalt nitrate, and dry at 80° C. for 5 hours.

[0062] 3. The sample obtained in (2) was transferred with 10 mL of carbon disulfide and sealed in a 60 mL autoclave in an argon atmosphere.

[0063] 4. React the autoclave in (3) at 400° C. for 9 hours.

[0064] 5. Treat the sample obtained in (4) with a 5% hydrofluoric acid solution by mass fraction for 8 hours, then wash with water, suction filter, and dry at 80° C. for 8 hours.

[0065] Transmission electron microscopy showed that the obtained sample had regular and uniform three-dimensional pores, and no metal particles were found. The X-ray diffraction spectrum shows that the obtained sample is composed of molybdenum disulfide and gr...

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Abstract

The invention discloses a preparation method of heteroatom doped porous molybdenum disulfide coated graphene. Specifically, the method comprises the following steps: wrapping a template agent with graphene oxide, with the mass ratio of the template agent to the graphene oxide being 20:1 to 1:10; then dispersing a metal ion salt on the abovementioned sample; carrying out a reaction with a sulfur-containing compound at a certain temperature; and finally removing the template agent to obtain the target product. The material prepared by the method has a regular spongy three-dimensional pore channel structure, and the outer walls of the graphene single pores are uniformly covered with heteroatom-doped molybdenum disulfide single pores. The material has high activity and good cycling stability when being used for an electrocatalytic hydrogen evolution reaction. The method is simple and easy to operate.

Description

technical field [0001] The invention relates to a preparation method of heteroatom-doped molybdenum disulfide-wrapped graphene. Background technique [0002] Molybdenum disulfide is a typical two-dimensional transition metal chalcogenide, which has received extensive attention because of its unique structure and electronic properties. It has broad application prospects in lubrication, hydrodesulfurization, photocatalysis and electrocatalysis. . In the electrocatalytic hydrogen evolution reaction, molybdenum disulfide is relatively inert in the two-dimensional plane, and the sides are active sites and have high catalytic activity. However, van der Waals forces inevitably exist between 2D MoS2 nanosheets, which make the nanosheets easy to fold and stack, resulting in the coverage of edge active sites. Based on the idea of ​​avoiding the active sites covered by molybdenum disulfide due to the stacking of nanosheets, Deng constructed a three-dimensional mesoporous molybdenum d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051B01J35/10C25B1/02C25B11/06
CPCB01J27/051B01J35/10B01J35/1061B01J35/1066C25B1/02C25B11/04
Inventor 邓德会孟祥宇包信和
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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