Preparation method of molybdenum disulfide nanotube and molybdenum disulfide nanotube

A molybdenum disulfide and nanotube technology, applied in the field of nanomaterials, can solve the problems of difficulty in controlling the diameter of MoS2 nanotubes and the thickness of the tube wall, and achieve the effects of easy removal, controllable wall thickness and uniform distribution.

Inactive Publication Date: 2021-04-06
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these methods can prepare MoS 2 Nanotubes, but hard to control MoS 2 Nanotube diameter and tube wall thickness
At the same time, it is also difficult for MoS 2 Nanotubes for large-scale industrial production

Method used

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  • Preparation method of molybdenum disulfide nanotube and molybdenum disulfide nanotube
  • Preparation method of molybdenum disulfide nanotube and molybdenum disulfide nanotube
  • Preparation method of molybdenum disulfide nanotube and molybdenum disulfide nanotube

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preparation example Construction

[0026] The steps of the preparation method of the present invention are:

[0027] After the commercial AAO template (aperture: 2-500nm, height: 100nm-500μm) is cleaned and plasma treated (time 1-30min), it is put into the cavity of a commercial atomic layer deposition equipment. In the ALD process, molybdenum pentachloride (MoCl 5 ) is molybdenum source, hydrogen sulfide (H 2 S) as a sulfur source, with nitrogen (N 2 ) as carrier and purge gas. Raise the temperature of the molybdenum source to 100-300°C to fully decompose and gasify the molybdenum source; keep the temperature of the ALD reaction chamber at 300-800°C. After reaching the required temperature, pass MoCl into the cavity according to this 5 (chemisorption on the surface of AAO via hydroxyl groups); N 2 (reaction residue and by-products are rinsed away); H 2 S (with MoCl 5 Reaction to generate MoS 2 ); N 2(Reaction residues and by-products are rinsed away). These four steps constitute an ALD cycle. Since t...

Embodiment 1

[0029] The AAO with a nanopore diameter of 200 nm and a height of 50 μm was cleaned, treated with plasma for 10 min, and then placed in an atomic layer deposition device. molybdenum pentachloride (MoCl 5 ) is molybdenum source, hydrogen sulfide (H 2 S) as a sulfur source, with nitrogen (N 2 ) as carrier and purge gas. Raise the temperature of the molybdenum source to 200°C; keep the temperature of the ALD reaction chamber at 500°C. After reaching the required temperature, pass MoCl into the cavity according to this 5 (flow rate: 50sccm; access time: 1s); N 2 (flow rate: 50sccm; access time: 30s); H 2 S (flow rate: 50sccm; access time: 1s); N 2 (flow rate: 50sccm; access time: 30s) as a cycle. In this way, cycled 50 times to get MoS 2 / AAO. Finally, the MoS 2 / AAO is immersed in sodium hydroxide (NaOH) solution, and the AAO template is etched away to obtain molybdenum disulfide nanotubes with a diameter of 200nm, a length of 50μm, and a wall thickness of 10nm.

Embodiment 2

[0031] The AAO with a nanopore diameter of 100 nm and a height of 20 μm was cleaned, treated with plasma for 5 minutes, and placed in an atomic layer deposition device. molybdenum pentachloride (MoCl 5 ) is molybdenum source, hydrogen sulfide (H 2 S) as a sulfur source, with nitrogen (N 2 ) as carrier and purge gas. Raise the temperature of the molybdenum source to 200°C; keep the temperature of the ALD reaction chamber at 500°C. After reaching the required temperature, pass MoCl into the cavity according to this 5 (flow rate: 50sccm; access time: 1s); N 2 (flow rate: 50sccm; access time: 30s); H 2 S (flow rate: 50sccm; access time: 1s); N 2 (flow rate: 50sccm; access time: 30s) as a cycle. In this way, cycled 50 times to get MoS 2 / AAO. Finally, the MoS 2 / AAO is immersed in sodium hydroxide (NaOH) solution, and the AAO template is etched away to obtain molybdenum disulfide nanotubes with a diameter of 100nm, a length of 20μm, and a wall thickness of 10nm.

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Abstract

The invention discloses a preparation method of a molybdenum disulfide nanotube, and the method comprises the following steps: by taking anodic aluminum oxide as a template, growing molybdenum disulfide with controllable thickness on the surface of a nanopore of the anodic aluminum oxide template by adopting an atomic layer deposition technology; and etching the anodic aluminum oxide by using an etching solution to obtain the MoS2 nanotube array. By selecting AAO templates with different pore diameters and heights and controlling the cycle number of ALD, the diameter, the length and the wall thickness of the MoS2 nanotube can be accurately regulated and controlled. The method solves the problem that the pipe diameter and the wall thickness of the molybdenum disulfide nanotube are uncontrollable, and the prepared molybdenum disulfide nanotube has good repeatability and orientation consistency, can be used in the fields of catalysis, semiconductors and the like, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of nanometer materials, and in particular relates to a preparation method of molybdenum disulfide nanotubes. Background technique [0002] MoS 2 (Molybdenum disulfide), as a typical layered two-dimensional material, has excellent mechanical properties (such as anti-friction, anti-oxidation), excellent photoelectric properties (such as tunable band gap) and excellent catalytic properties. (such as electrocatalytic hydrogen evolution), etc., have attracted widespread attention. In order to further improve the MoS 2 Excellent performance and expanded application fields, MoS with various morphologies 2 Has been prepared, such as sheet, coral, hollow spherical, core-shell, rod and so on. Among them, tubular MoS 2 Due to its unique physical and chemical properties, it has attracted extensive attention. Tubular MoS 2 First through MoO 3 and H 2 S is obtained by gas-phase reaction at high temperature (800-950 °C) in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B82Y30/00B82Y40/00
CPCC01G39/06B82Y30/00B82Y40/00C01P2004/13C01P2004/03
Inventor 刘磊焦松龙吕俊孔孟书
Owner SOUTHEAST UNIV
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