Sodium chloride-assisted method for growth of multilayer transition metal chalcogenides

A technology of chalcogen compounds and transition metals, applied in the field of materials, can solve the problems of high growth temperature, uncontrollable layer number, long growth time, etc., and achieve the effect of efficient growth and controllable preparation

Active Publication Date: 2019-02-01
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the current preparation process of transition metal chalcogenide chemical vapor deposition, there are still problems such as uncontrollable layer number, long growth time, and high growth temperature.

Method used

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  • Sodium chloride-assisted method for growth of multilayer transition metal chalcogenides
  • Sodium chloride-assisted method for growth of multilayer transition metal chalcogenides
  • Sodium chloride-assisted method for growth of multilayer transition metal chalcogenides

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Clean the purchased soda-lime glass (5cm×5cm, thickness 2mm) by placing the soda-lime glass in deionized water (18.2MΩ·cm), acetone (analytical grade) and isopropanol (analytical grade) in sequence. ) for 10 minutes of ultrasonic cleaning, followed by drying with high-purity nitrogen to complete the cleaning. Put the cleaned soda-lime glass on the graphite boat, place a molybdenum foil with the same size as the substrate 10mm above the graphite boat, place them together in a high-temperature tubular reactor, and place elemental sulfur powder at 15cm upstream of the airflow relative to the substrate 150 g, and feed high-purity argon (50 sccm) to flush the reaction chamber for 10 minutes to remove residual air in the chamber. Introduce a certain amount of oxygen (3 sccm) and then start the heating program to heat the reaction chamber. The final temperatures of the sulfur powder and the substrate are 100°C and 750°C respectively, the heating time is 35 minutes, and the tem...

Embodiment 2

[0038] Clean the purchased soda-lime glass (5cm×5cm, thickness 2mm) by placing the glass in deionized water (18.2MΩ·cm), acetone (analytical grade) and isopropanol (analytical grade) in sequence Ultrasonic cleaning was performed for 10 minutes, followed by drying with high-purity nitrogen to complete the cleaning. Place the cleaned soda-lime glass on a graphite boat. Sodium chloride granules were dissolved in ultrapure water to prepare a certain concentration of sodium chloride solution (0.01mmol / L, 0.02mmol / L, 0.03mmol / L, respectively). Immerse the molybdenum or tungsten foil in the solution, take it out slowly after 10 minutes, and let it dry naturally. The molybdenum foil coated with sodium chloride is placed 10mm above the graphite boat, and placed together in a high-temperature tubular reactor, 50g of elemental sulfur powder is placed at 15cm upstream of the airflow relative to the substrate, and high-purity argon gas ( 50 sccm) to flush the reaction chamber for 10 minu...

Embodiment 3

[0041] Raman spectroscopy (excitation wavelength is 532nm) and fluorescence spectroscopy were used to characterize the optical properties of molybdenum disulfide layers with or without sodium chloride assisted growth in Examples 1 and 2. Depend on image 3From the results of Raman spectroscopy, it can be seen that two characteristic peaks of molybdenum disulfide can be observed in samples with different layers, indicating that the synthesized samples are all molybdenum disulfide. As the molybdenum disulfide changes from a single layer to a multilayer, the Raman characteristic peak spacing gradually increases, which is consistent with the Raman change characteristics of molybdenum disulfide with different layers.

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Abstract

The invention discloses a sodium chloride-assisted method for growth of multilayer transition metal chalcogenides. The method comprises the following steps: 1) cleaning a substrate, and placing the substrate to a graphite boat; 2) preparing a certain concentration of a sodium chloride solution, immersing a molybdenum foil or tungsten foil into the solution, taking out the molybdenum foil or tungsten foil after several minutes, and naturally airing; 3) placing the sodium chloride-loaded molybdenum foil or tungsten foil to the graphite boat for holding the substrate; 3) placing elemental sulfurat the upstream of the substrate; and 4) introducing argon and oxygen until the airflow is stable, respectively heating the substrate and the elemental sulfur to different temperatures until reachinga constant temperature, and growing layers-controllable multilayer transition metal chalcogenides on the substrate after several minutes. By the sodium chloride-assisted method for growth of multilayer transition metal chalcogenides, the layers-controllable multilayer sample can be obtained by controlling quality of sodium chloride. The method is a method for efficient preparation of high-qualitymultilayer transition metal sulfides.

Description

technical field [0001] The invention belongs to the field of materials. Specifically, the invention relates to the method of using low-pressure chemical vapor deposition, with the assistance of sodium chloride, to efficiently prepare multilayer transition metal chalcogen compounds such as molybdenum disulfide and tungsten disulfide with a controllable number of layers . Background technique [0002] Two-dimensional layered transition metal chalcogenides (MX 2 ,M=Mo,W; X=S,Se), as a class of graphene-like materials, has great applications in the fields of high-frequency photodetection and sensing due to its unique layer number-dependent optical and electronic properties. prospect. At present, there are many ways to control the optical and electrical properties of such devices, such as using stress, external electric field and chemical doping, etc. However, the two-dimensional layered nature of transition metal chalcogenides provides people with a unique control means, that...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06C01G41/00
CPCC01G39/06C01G41/00C01P2004/20
Inventor 张艳锋杨鹏飞张哲朋
Owner PEKING UNIV
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