CN113816426A - Two-dimensional material crystal structure regulation and control method induced by electron beam irradiation - Google Patents

Two-dimensional material crystal structure regulation and control method induced by electron beam irradiation Download PDF

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Publication number
CN113816426A
CN113816426A CN202111202714.7A CN202111202714A CN113816426A CN 113816426 A CN113816426 A CN 113816426A CN 202111202714 A CN202111202714 A CN 202111202714A CN 113816426 A CN113816426 A CN 113816426A
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China
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dimensional material
electron beam
layer
crystal structure
irradiation
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徐涛
朱亚彤
国洪轩
孙立涛
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Southeast University
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Southeast University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/007—Tellurides or selenides of metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like

Abstract

The invention discloses a method for regulating and controlling a two-dimensional material crystal structure induced by electron beam irradiation, which comprises the following steps: step 1, preparing a single-layer or few-layer two-dimensional material; 2, placing a single-layer or few-layer two-dimensional material on a sample carrying table, and continuously heating for 8-12 hours under a vacuum condition; step 3, placing the single-layer or few-layer two-dimensional material in a high-energy electron beam radiation environment to obtain a regulated two-dimensional material; wherein, the adopted irradiation equipment is a transmission electron microscope, and the visual monitoring of the regulation and control process is realized in an atomic scale at the same time of irradiation treatment; the energy range of the high-energy electron beam in the high-energy electron beam radiation environment is 60 keV-300 keV, and the dose rate range is 104～109e‑·nm‑2·s‑1. The invention relates to a two-dimensional material crystal structure regulating and controlling methodThe method has better flexibility, can be used for preparing a two-dimensional heterostructure and is suitable for preparing a two-dimensional device.

Description

Two-dimensional material crystal structure regulation and control method induced by electron beam irradiation
Technical Field
The invention belongs to the field of nano processing technology and nano devices, and particularly relates to a method for regulating and controlling a two-dimensional material crystal structure induced by electron beam irradiation.
Background
With the continuous acceleration of the miniaturization process of electronic devices, the semiconductor industry has entered the next Moore era. In order to obtain a device with smaller size and higher integration level, the top-down micro-nano manufacturing process needs to develop a processing technology with smaller line width to realize the construction of a nano-or even sub-nano characteristic width structure. On the other hand, the limitation of the traditional design idea is broken through, and the development of novel devices by utilizing and regulating the quantum effect becomes an important direction for the development of the semiconductor industry. An 2015-version international technical roadmap for semiconductors indicates that a two-dimensional material with the characteristics of ultrathin channels, high mobility, controllable energy bands and the like is expected to become an important basic electronic material in the post-molars era and plays an important role in the design of novel devices.
The singular nature of a two-dimensional material depends to a large extent on the crystal structure of the material (arrangement of atoms in plane, number of layers, stacking, etc.). In addition, due to the structural characteristics of two-dimensional materials, the arrangement of atoms has a more significant influence on the physical properties of the materials than three-dimensional bulk materials. Therefore, it is important to construct a two-dimensional material with unique properties by atomic structure control to meet the increasing application requirements.
Although the control of the two-dimensional material macro-crystal structure and performance can be realized in multiple ways in the material preparation process, the exploration and research and development of a novel device based on the two-dimensional material needs a processing technology to realize the local structure control of nano-scale and precision. The highest accelerating voltage of the current electron beam processing system is 30-100 kV, the minimum beam spot is 3-5nm, and the regulation and control capability and the precision of the two-dimensional material local structure phase change in the processing process are limited.
Disclosure of Invention
The invention aims to provide a two-dimensional material crystal structure regulating and controlling method induced by electron beam irradiation, and aims to solve the technical problem that the regulating and controlling capability and the precision of the existing electron beam processing system on the local structure phase change of a two-dimensional material are limited in the processing process.
In order to solve the technical problems, the specific technical scheme of the invention is as follows:
a method for regulating and controlling a two-dimensional material crystal structure induced by electron beam irradiation comprises the following steps:
step 1, preparing a single-layer or within 10-layer two-dimensional material;
2, placing a single-layer or few-layer two-dimensional material on a sample carrying table, and continuously heating for 8-12 hours under a vacuum condition;
step 3, placing the single-layer or few-layer two-dimensional material in a high-energy electron beam radiation environment to obtain a regulated two-dimensional material; wherein, the adopted irradiation equipment is a transmission electron microscope, and the visual monitoring of the regulation and control process is realized in an atomic scale at the same time of irradiation treatment;
the energy range of the high-energy electron beam in the high-energy electron beam radiation environment is 60 keV-300 keV, and the dose rate range is 104～109e-·nm-2·s-1。
Further, the two-dimensional material in step 1 comprises molybdenum disulfide, tungsten disulfide, molybdenum diselenide or diselenide.
Further, the heating temperature range involved in the step 2 is 70-200 ℃.
Further, the preparation method in step 1 is a micro-mechanical lift-off method.
The method for regulating and controlling the crystal structure of the two-dimensional material induced by electron beam irradiation has the following advantages:
1. the invention can controllably induce the change of the crystal structure of the two-dimensional material by utilizing the electron beam with the high energy range of 60keV to 300keV to form a new structural phase;
2. the invention adopts the transmission electron microscope, can realize the visual monitoring of the regulation and control process in the atomic scale at the same time of irradiation treatment, and has flexibility.
Drawings
FIG. 1 is a schematic diagram of electron beam irradiation induced two-dimensional material crystal structure modulation of the present invention;
FIG. 2(a) shows a two-dimensional material WSe according to the present invention2Microscopic image before irradiation;
FIG. 2(b) shows a two-dimensional material WSe according to the present invention2On spokeA pre-illumination magnified microscopic image;
FIG. 2(c) shows a two-dimensional material WSe according to the present invention2Microscopic image after irradiation;
FIG. 2(d) shows a two-dimensional material WSe according to the present invention2A magnified microscopic image of the phase change region after irradiation;
FIG. 3(a) shows a two-dimensional material WSe according to the present invention2A fast Fourier transform image corresponding to the microscopic image before irradiation;
FIG. 3(b) shows a two-dimensional material WSe according to the present invention2And (3) generating a fast Fourier transform image corresponding to the microscopic image of the phase change region after irradiation.
Detailed Description
In order to better understand the purpose, structure and function of the present invention, the following describes the method for regulating and controlling the crystal structure of two-dimensional material induced by electron beam irradiation in further detail with reference to the accompanying drawings.
A method for regulating and controlling a two-dimensional material crystal structure induced by electron beam irradiation comprises the following steps:
step 1, preparing a single-layer or less than 10-layer two-dimensional material; the two-dimensional material comprises molybdenum disulfide, tungsten disulfide, molybdenum diselenide or diselenide, and the preparation method is a micromechanical stripping method.
And 2, placing the single-layer or few-layer two-dimensional material on a sample carrying table, and continuously heating for 8-12 hours under a vacuum condition, wherein the related heating temperature range is 70-200 ℃.
Step 3, placing the single-layer or few-layer two-dimensional material in a high-energy electron beam radiation environment to obtain a regulated two-dimensional material; wherein, the adopted irradiation equipment is a transmission electron microscope, and the visual monitoring of the regulation and control process is realized in an atomic scale at the same time of irradiation treatment;
the energy range of the high-energy electron beam in the high-energy electron beam radiation environment is 60 keV-300 keV, and the dose rate range is 104～109e-·nm-2·s-1。
A first embodiment of the invention comprises the steps of:
the first step is as follows: using micromechanical stripping methodsSlave WSe2Stripping off few layers of WSe in the block2；
The second step is that: will have few layers WSe2Transferring to a transmission electron microscope carrier net, and then heating to 70 ℃ on a vacuum heating table for 12 hours; placing the carrier net on a transmission electron microscope sample stage and inserting the carrier net into the transmission electron microscope;
the third step: will have few layers WSe2Exposed to an electron beam environment at an energy of 300keV and a dose rate of 108e-·nm-2·s-1And the duration was 30 minutes.
The results are shown in FIGS. 2 and 3.
FIG. 2(a) shows a two-dimensional material WSe according to the present invention2Microscopic image before irradiation, FIG. 2(b) is a two-dimensional material WSe of the present invention2A magnified microscopic image before irradiation; FIG. 2(c) shows a two-dimensional material WSe according to the present invention2Microscopic image after irradiation; FIG. 2(d) shows a two-dimensional material WSe according to the present invention2A magnified microscopic image of the phase change region after irradiation; FIG. 3(a) shows a two-dimensional material WSe according to the present invention2A fast Fourier transform image corresponding to the microscopic image before irradiation; FIG. 3(b) shows a two-dimensional material WSe according to the present invention2And a fast Fourier transform image corresponding to the microscopic image of the phase change area after irradiation can visually reflect the generation of phase change. In addition, the regulation and control process is visual, the generation of phase change and the change of the area of a phase change area can be monitored in real time, and the real-time monitoring and regulation and control of the material structure are realized.
It is to be understood that the present invention has been described with reference to certain embodiments, and that various changes in the features and embodiments, or equivalent substitutions may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (4)

1. A method for regulating and controlling a two-dimensional material crystal structure induced by electron beam irradiation is characterized by comprising the following steps:
step 1, preparing a single-layer or within 10-layer two-dimensional material;
2, placing a single-layer or few-layer two-dimensional material on a sample carrying table, and continuously heating for 8-12 hours under a vacuum condition;
step 3, placing the single-layer or few-layer two-dimensional material in a high-energy electron beam radiation environment to obtain a regulated two-dimensional material; wherein, the adopted irradiation equipment is a transmission electron microscope, and the visual monitoring of the regulation and control process is realized in an atomic scale at the same time of irradiation treatment;
the energy range of the high-energy electron beam in the high-energy electron beam radiation environment is 60 keV-300 keV, and the dose rate range is 104～109e-·nm-2·s-1。
2. The method for regulating and controlling the crystal structure of the two-dimensional material induced by the electron beam irradiation as claimed in claim 1, wherein the two-dimensional material in the step 1 comprises molybdenum disulfide, tungsten disulfide, molybdenum diselenide or diselenide.
3. The method for regulating and controlling the crystal structure of the two-dimensional material induced by the electron beam irradiation according to claim 1, wherein the heating temperature range involved in the step 2 is 70-200 ℃.
4. The method for regulating and controlling the crystal structure of the two-dimensional material induced by the electron beam irradiation according to claim 1, wherein the preparation method in the step 1 is a micro-mechanical peeling method.
CN202111202714.7A 2021-10-15 2021-10-15 Two-dimensional material crystal structure regulation and control method induced by electron beam irradiation Pending CN113816426A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030155523A1 (en) * 2001-04-03 2003-08-21 Ki-Bum Kim Apparatus and a method for forming a pattern using a crystal structure of material
CN109830533A (en) * 2019-01-30 2019-05-31 上海电力学院 A kind of field effect transistor based on two-dimensional material preparation
CN110646490A (en) * 2019-09-30 2020-01-03 深圳大学 Ion sensitive field effect transistor sensor based on tungsten diselenide and preparation method thereof
CN111690897A (en) * 2020-06-23 2020-09-22 南京大学 Tungsten diselenide thin film of single primitive cell layer and growth method thereof
CN111792622A (en) * 2020-09-10 2020-10-20 西湖大学 Water ice-based electron beam induced etching process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030155523A1 (en) * 2001-04-03 2003-08-21 Ki-Bum Kim Apparatus and a method for forming a pattern using a crystal structure of material
CN109830533A (en) * 2019-01-30 2019-05-31 上海电力学院 A kind of field effect transistor based on two-dimensional material preparation
CN110646490A (en) * 2019-09-30 2020-01-03 深圳大学 Ion sensitive field effect transistor sensor based on tungsten diselenide and preparation method thereof
CN111690897A (en) * 2020-06-23 2020-09-22 南京大学 Tungsten diselenide thin film of single primitive cell layer and growth method thereof
CN111792622A (en) * 2020-09-10 2020-10-20 西湖大学 Water ice-based electron beam induced etching process

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
KAMYAR PARTO ET AL.: "Defect and strain engineering of monolayer WSe2 enables site-controlled single-photon emission up to 150K" *
徐涛: "新型二维材料电子辐照效应研究" *
徐涛等: "二维层状材料原位电子辐照研究" *

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