A method for preparing large-scale single-crystal two-dimensional materials based on chemical vapor deposition

A technology of chemical vapor deposition and two-dimensional materials, which is applied in the field of preparing large-size single-crystal two-dimensional materials based on chemical vapor deposition, can solve the problems of difficult formation of single-crystal structures and low quality of large-size single-crystal two-dimensional materials, and reduce the The effect of preparation cost, simplification of material types, and promotion of interaction

Active Publication Date: 2022-07-26
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Either in H 2 Whether Ar is used as the carrier gas, the material interaction of the growth system is only studied, and the nucleation and growth process of two-dimensional materials not only depends on the interaction between substances, but is the result of the joint influence of multiple factors. From a single Adjusting the angle will lead to low quality of large-size single-crystal two-dimensional materials, and it is difficult to form a uniform single-crystal structure. The quality of single-crystal 2D materials, obtaining large-scale 2D structures of single crystals

Method used

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  • A method for preparing large-scale single-crystal two-dimensional materials based on chemical vapor deposition
  • A method for preparing large-scale single-crystal two-dimensional materials based on chemical vapor deposition
  • A method for preparing large-scale single-crystal two-dimensional materials based on chemical vapor deposition

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preparation example Construction

[0073] The Si / SiO 2 The preparation method of the substrate is: evaporating SiO from a commercial Si wafer 2 layer, and for evaporation of SiO 2 One side of the layer is polished to serve as a substrate.

[0074] Further, SiO 2 The thickness of the layer is 200-300 nm;

[0075] Further, the distance between the different temperature zones is 15-20cm;

[0076] (2) Vacuum flush the furnace cavity with inert gas;

[0077] Further, the furnace cavity is evacuated, and inert gas is introduced to the furnace cavity pressure of 0.5-1 atm, then the furnace cavity is evacuated, and the operation is repeated to perform vacuum treatment on the furnace cavity;

[0078] Further, during the vacuum flushing process of the furnace cavity, the number of repetitions is 3 to 5 times to fully ensure that there is no oxygen, water vapor and other gases unrelated to the reaction in the furnace cavity.

[0079] (3) The temperature in different temperature zones is heated up respectively, and t...

Embodiment 1

[0089] A method for preparing a large-sized single crystal two-dimensional graphene material, comprising the following steps:

[0090] (1) Select metal copper Cu as the substrate, and carry out pretreatment such as cleaning, electrochemical polishing, and oxidation;

[0091] (2) Place the pretreated Cu substrate in the reaction furnace chamber, and then evacuate the furnace chamber to 5×10 -5 Pa; close the vacuum pump unit, introduce inert gas Ar to the furnace chamber pressure of 1 atm, then turn on the vacuum pump unit, pump and charge the furnace chamber, repeat 3 times, and vacuum the furnace chamber;

[0092](3) Raise the temperature of the equipment to 1050°C, compare with H 2 Add changes to the temperature field. Into the furnace cavity and Ar 2 (500sccm) and H 2 (10sccm) mixed gas was used as the carrier gas, the furnace chamber was adjusted to the target pressure of 0.75 atm, and the substrate was annealed for 60 min. Under this condition, the temperature field i...

Embodiment 2

[0104] A kind of preparation of large-size single crystal two-dimensional MoSe 2 The method of the material includes the following steps:

[0105] (1) Evaporate 300nm thick SiO on a commercial Si wafer 2 layer, and for evaporation of SiO 2 One side of the layer is polished as a substrate;

[0106] (2) Treated Si / SiO 2 The substrate is placed in the furnace chamber, and the polished surface is aligned with the MoO 3 Precursor; Se powder precursor is placed before the substrate with a distance of 20cm;

[0107] (3) Then the furnace cavity is evacuated, and the vacuum degree is not higher than 5×10 -5 Pa; turn off the vacuum pump unit, introduce inert background gas to the furnace chamber pressure of 1 atm, then turn on the vacuum pump unit, pump and charge the furnace chamber, repeat 3 times, and vacuum the furnace chamber;

[0108] (4) Set the programmed heating respectively, the temperature of the Se region is raised to 250°C, and the heating rate is 10°C / min; Si / SiO 2 ...

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Abstract

The invention belongs to the field of two-dimensional material preparation, and in particular relates to a method for preparing large-size single-crystal two-dimensional materials based on chemical vapor deposition. The method is as follows: using a mixture of carrier gas A and carrier gas B as the carrier gas, first constructing a nearly flat and slightly convex temperature field by setting the ratio of carrier gas A and carrier gas B, and then adjusting the ratio of the two to construct a flat and flat temperature field. A large-size single-crystal two-dimensional material is obtained through chemical vapor deposition; the carrier gas A is an inert gas, and the carrier gas B is a gas with different thermal conductivity from the carrier gas A. By introducing into the reaction chamber gas that does not participate in the chemical reaction of two-dimensional materials and has different thermal conductivity, the invention can effectively regulate the temperature field in the reaction chamber while strengthening the interaction between substances, and design and realize the two-dimensional material in the reaction chamber. The transition from the convex temperature field to the flat temperature field in the material growth region fully provides the temperature driving force, which in turn promotes the lateral growth of the core of the two-dimensional material, and finally obtains a high-quality large-size single-crystal two-dimensional material.

Description

technical field [0001] The invention belongs to the field of two-dimensional material preparation, in particular to a method for preparing large-size single-crystal two-dimensional materials based on chemical vapor deposition. Background technique [0002] The information disclosed in this Background section is only for enhancement of understanding of the general background of the invention and should not necessarily be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art. [0003] The successful preparation of graphene in 2005 broke the theory that two-dimensional materials are thermodynamically unstable and cannot exist. In recent years, with the further development of scientific research, new two-dimensional layered materials have been continuously discovered, and they have exhibited unique electrical, optical, magnetic and other physical properties, showing great potential i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B25/02C30B25/14
CPCC30B25/02C30B25/14
Inventor 赵显孙丽王鹏国星张雪李妍璐于法鹏
Owner SHANDONG UNIV
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