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Method for preparing orthogonal-phase MoO3 monocrystal nanosheet through chemical vapor deposition

A chemical vapor deposition and single-crystal nanotechnology, which is applied in the field of nanomaterials, can solve the problem of liquid phase process safety and acidification operation is difficult to control, affecting the intrinsic physical properties of α-MoO nanocrystals, and the nanostructure morphology and size are not uniform, etc. problems, to achieve the effect of safe and non-toxic preparation process, superior crystallinity and single crystal quality, single raw material and equipment

Inactive Publication Date: 2015-06-24
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the MoO obtained by the liquid phase method 3 The morphology and size of nanostructures are not uniform enough, and the existence of various chemical groups in the growth environment makes the extrinsic defect states, surface states and other microstructural features of the sample complex, which cannot form perfect crystallinity and single crystal characteristics, affecting α-MoO 3 Intrinsic physical properties of nanocrystals, and there are problems in the liquid phase process, such as safety and acidification operation are not easy to control
[0007] Direct Preparation of α-MoO on Silicon Substrates by Pulsed Electron Beam Deposition and Pulsed Laser Deposition 3 Nanorod arrays, however, they require expensive deposition equipment, high vacuum requirements, strict control of preparation process conditions, high energy consumption, and low yield, which restricts the application of industrial mass production

Method used

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  • Method for preparing orthogonal-phase MoO3 monocrystal nanosheet through chemical vapor deposition
  • Method for preparing orthogonal-phase MoO3 monocrystal nanosheet through chemical vapor deposition
  • Method for preparing orthogonal-phase MoO3 monocrystal nanosheet through chemical vapor deposition

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Experimental program
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Embodiment 1

[0029] α-MoO 3 The preparation method of single crystal nanosheet comprises the following steps:

[0030] Step 1. Select a 2cm×3cm quartz plate as the sample deposition substrate, and clean the surface of the substrate before deposition and growth. The specific scheme is: put the substrate into acetone for 15 minutes, then put it into ethanol for 15 minutes, and finally clean it in ionized water for 10 minutes, take out the cleaned quartz substrate, and dry it with nitrogen.

[0031] Step 2. Take MoS 2 Put 0.2g of powder into the ceramic boat as a raw material, place the ceramic boat with the raw material in the quartz tube of the tube furnace, and place the cleaned quartz substrate on the downwind port of the ceramic boat (the carrier gas flows into the ceramic boat from the air inlet). , carrying the sublimated Mo gas source to the oxidation crystal at the substrate through the high-temperature ceramic boat, and the carrier gas is discharged from the other end of the gas o...

Embodiment 2

[0039] In the above step 5, the reaction temperature of the tube furnace is set at 600-700° C., and the holding time is 20 min. Other steps and details remain unchanged from Example 1.

[0040]The sample prepared in Example 2 is not a uniform orthorhombic cubic crystal system, but has monoclinic and hexagonal crystal systems, so MoO with a uniform orthorhombic cubic crystal phase cannot be formed at a reaction temperature lower than 700°C. 3 crystals.

Embodiment 3

[0042] In step 5 of embodiment 1, the reaction time of setting the tube furnace is 30-40min, and other steps and details remain unchanged from embodiment 1.

[0043] The sample prepared in Example 3 still maintains a uniform orthorhombic cubic crystal system without the existence of monoclinic and hexagonal crystal systems, but the thickness of the nanosheets increases significantly, so the deposition and growth time can effectively control the two-dimensional nanosheets thickness of.

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Abstract

The invention relates to a method for preparing an orthogonal-phase MoO3 monocrystal nanosheet through chemical vapor deposition, which comprises the following steps: cleaning a quartz substrate, sequentially performing ultrasonic cleaning in acetone, ethanol and deionized water, and blow-drying with nitrogen gas; placing 0.2-0.5g of MoS2 powder into a ceramic boat, and putting into a quartz tube of a tube furnace; putting the quartz substrate at the downwind opening of the ceramic boat filled with the raw material, sealing the tube furnace, and introducing argon to wash the tube furnace; and after cleaning, introducing argon and oxygen mixed gas, turning on a vacuum mechanical pump, starting a tube furnace heating program to raise the temperature, then naturally cooling to room temperature, and taking out a sample, wherein a white product is grown on the quartz substrate and is the monocrystal MoO3 nanosheet. The invention overcomes the respective defects in wet chemical stripping, a microwave method and a hydrothermal method. According to the invention, preparation technology of alpha-MoO3 nanocrystal is expanded; the synthesis process is simple and easy to control; the used raw materials and equipment are simplex and cheap; the preparation flow is safe, non-toxic, quick and efficient; and the obtained sample is high in yield.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, in particular to the preparation of orthorhombic MoO by chemical vapor deposition 3 Single Crystal Nanosheet Method. Background technique [0002] MoO 3 There are three common crystal phase structures: thermodynamically stable orthorhombic phase (α-MoO 3 ) and thermodynamically metastable monoclinic phase (β-MoO 3 ) and hexagonal phase (h-MoO 3 ). where α-MoO 3 Belonging to wide bandgap semiconductors (E g =3.05eV), which is caused by the distorted [MoO 6 ] The octahedrons are connected by common edges in one direction, and connected by common vertices in the other direction, forming a two-dimensional infinitely stretched plane layer, and the layers are combined by weak van der Waals force. Two-dimensional Quantum Strong Confinement α-MoO 3 The nanosheet structure has remarkable photoluminescence, field emission, reversible photochromism, photochromism, electrochromism, gas sensing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/16C30B29/64C30B25/00
CPCC30B29/16C30B25/00C30B29/64
Inventor 许小勇周钢冯兵王亚丽包志佳胡经国
Owner YANGZHOU UNIV
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