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A kind of molybdenum disulfide with three-dimensional hierarchical porous structure and its preparation method and application

A technology of molybdenum disulfide and hierarchical pores, which is applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of disordered overall structure, collapse of pore structure, easy agglomeration, etc. Easy agglomeration and deactivation, stable pore structure, and improved specific surface area

Active Publication Date: 2022-03-11
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, the control of the hierarchical pore structure of molybdenum disulfide has not been effectively reported. However, according to the reported preparation methods of the hierarchical pore structure of other materials, it can be seen that when adjusting the pore structure of a scale, often Make the pore structure of another scale collapse and break up, and then the overall structure becomes disordered and easy to agglomerate
Therefore, how to effectively adjust the scale and proportion of each template to form a three-dimensional hierarchical porous structure of molybdenum disulfide is still a huge challenge.

Method used

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  • A kind of molybdenum disulfide with three-dimensional hierarchical porous structure and its preparation method and application
  • A kind of molybdenum disulfide with three-dimensional hierarchical porous structure and its preparation method and application
  • A kind of molybdenum disulfide with three-dimensional hierarchical porous structure and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. Take 1.9g of silicon dioxide (100nm) and 0.9g of silicon dioxide (20nm) and ultrasonically disperse in ethylene glycol solution for 3h, then stir at 50°C for 24h, dry at 100°C for 12h, take out and grind for 0.3 After h, the template A is obtained.

[0046] 2. Dissolve 400mg of ammonium molybdate in 30mL of water, add template A, mix with ultrasound for 1h, stir at room temperature for 24h, then dry at 60°C for 12h, then seal with 10mL of carbon disulfide in a 60mL autoclave under argon protection middle.

[0047] 3. Keep the autoclave in (2) at 200°C for 4h.

[0048] 4. Seal the sample obtained in (3) in 10% hydrofluoric acid solution and let it stand for 12 hours. Then wash with ultrapure water and ethanol several times and filter with suction.

[0049] 5. Dry the sample obtained in (4) at 100°C for 12 hours to obtain a three-dimensional hierarchical porous structure molybdenum disulfide, named 100nm / 20nm-MoS 2 .

[0050] TEM (see figure 1 ) shows that the ob...

Embodiment 2

[0052] 1. Take 1.2g of silicon dioxide (200nm) and 0.5g of silicon dioxide (10nm) and ultrasonically disperse in ethylene glycol solution for 3h, then stir at 50°C for 24h, dry at 100°C for 12h, take out and grind for 0.3 After h, the template A is obtained.

[0053] 2. Dissolve 400mg of ammonium molybdate in 30mL of water, add template A, ultrasonically mix for 1h, stir at room temperature for 24h, then dry at 60°C for 12h, then seal with 10mL of carbon disulfide in a 60mL autoclave under argon protection middle.

[0054] 3. Keep the autoclave in (2) at 200°C for 4h.

[0055] 4. Seal the sample obtained in (3) in 10% hydrofluoric acid solution and let it stand for 12 hours. Then wash with ultrapure water and ethanol and filter with suction.

[0056] 5. Dry the sample obtained in (4) at 100°C for 12 hours to obtain a three-dimensional hierarchical porous structure molybdenum disulfide, named 200nm / 10nm-MoS 2 .

[0057] TEM (see image 3 ) shows that the obtained sample i...

Embodiment 3

[0059] 1. Take 1.2g of silicon dioxide (400nm) and 0.2g of silicon dioxide (70nm) and ultrasonically disperse in ethylene glycol solution for 3h, then stir at 50°C for 24h, dry at 100°C for 12h, take out and grind for 0.3 After h, the template A is obtained.

[0060] 2. Dissolve 400mg of ammonium molybdate in 30mL of water, add template A, ultrasonically mix for 1h, stir at room temperature for 24h, then dry at 60°C for 12h, then seal with 10mL of carbon disulfide in a 60mL autoclave under argon protection middle.

[0061] 3. Keep the autoclave in (2) at 300°C for 4h.

[0062] 4. Seal the sample obtained in (3) in 10% hydrofluoric acid solution and let it stand for 12 hours. Then wash with ultrapure water and ethanol and filter with suction.

[0063] 5. Dry the sample obtained in (4) at 100°C for 12 hours to obtain a three-dimensional hierarchical porous structure molybdenum disulfide, named 400nm / 70nm-MoS 2 .

[0064] SEM (see Figure 5 ) shows that the obtained sample ...

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Abstract

The invention discloses a method for preparing molybdenum disulfide with a three-dimensional hierarchical porous structure. Specifically, the method first prepares templates of various scales, then thoroughly mixes the molybdenum-based compound with the template, reacts with the sulfur-containing compound at a certain temperature, and finally undergoes solution treatment, suction filtration and drying to obtain the target product. The material prepared by the method has a complete three-dimensional multi-level pore structure without clusters and collapse phenomenon, and the pore wall is composed of molybdenum disulfide nanosheet arrays. The types of templates used and the dimensions of the pores are easy to adjust. The material has excellent activity for electrocatalytic hydrogen evolution reaction. This method is a universal method for molybdenum disulfide with three-dimensional hierarchical porous structure, and has the characteristics of simplicity and easy operation.

Description

technical field [0001] The invention belongs to the field of nanometer two-dimensional materials, and in particular relates to a three-dimensional multi-level porous structure molybdenum disulfide and its preparation method and application. Background technique [0002] Two-dimensional molybdenum disulfide has attracted extensive attention in the field of catalysis including electrocatalysis, photocatalysis and traditional catalysis due to its unique structure and electronic properties. At the same time, its advantages such as large natural reserves, low price, and superior performance make molybdenum disulfide a promising substitute for noble metal hydrogen evolution electrocatalysts. At present, the hydrogen evolution active sites of molybdenum disulfide mainly come from its small amount of edge sulfur sites, while a large number of sulfur sites in its plane are relatively inert (B.Hinnemann, J.K. al. J. Am. Chem. Soc., 127, 5308-5309 (2005)). Moreover, due to the van d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/051C25B11/075C25B11/04
CPCB01J27/051C25B1/04C25B11/04B01J35/33B01J35/40B01J35/60Y02E60/36
Inventor 邓德会郑智龙胡景庭孟祥宇
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI