CN110923663A - Method for growing large-area single-layer or multi-layer molybdenum ditelluride structure through secondary reaction - Google Patents
Method for growing large-area single-layer or multi-layer molybdenum ditelluride structure through secondary reaction Download PDFInfo
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- CN110923663A CN110923663A CN201911093705.1A CN201911093705A CN110923663A CN 110923663 A CN110923663 A CN 110923663A CN 201911093705 A CN201911093705 A CN 201911093705A CN 110923663 A CN110923663 A CN 110923663A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
Abstract
The invention discloses a method for growing a large-area single-layer or multi-layer molybdenum ditelluride structure by secondary reaction. The method comprises the steps of firstly depositing a molybdenum telluride nano film on a substrate in an atomic layer deposition mode, and then carrying out high-temperature secondary reaction on the substrate on which the molybdenum telluride nano film is deposited and elemental tellurium by taking inert gas or hydrogen as carrier gas to obtain a large-area single-layer or multi-layer molybdenum ditelluride structure on the substrate. The invention has the advantages that: good controllability and simple operation, and can realize large-area preparation of single-layer or multi-layer molybdenum ditelluride. The molybdenum ditelluride structure prepared by the method has wide application prospect in the aspects of optical materials, storage materials, catalytic materials, semiconductor photoelectric materials and the like.
Description
Technical Field
The invention belongs to the field of material preparation, relates to a vapor deposition technology, and particularly relates to a method for growing a large-area single-layer or multi-layer molybdenum ditelluride structure through secondary reaction.
Background
Since Novoseov and Geim and their co-workers successfully used adhesive tapes to strip graphene from graphite in 2004, research on two-dimensional materials has entered a period of rapid development, and at the same time, graphene and graphene-like materials have further enriched families of two-dimensional materials, such as two-dimensional transition metal chalcogenides, particularly molybdenum ditelluride, and have a wide application prospect in the aspects of optical materials, storage materials, catalytic materials, semiconductor photoelectric materials and the like due to their excellent electrical, optical and mechanical properties.
Although two-dimensional nanomaterials show attractive prospects, the bottleneck that restricts the development of the nanomaterials is how to prepare high-quality large-area two-dimensional materials on a large scale. The preparation methods of the two-dimensional nano materials commonly used at present can be classified into two main types: a top-down stripping method and a bottom-up synthesis method. The top-down peeling method is the most traditional method for preparing two-dimensional materials, the preparation method is simple, the obtained samples have few defects, but the yield is low, and the method is not suitable for large-area production. The bottom-up synthesis method is mainly characterized in that a molybdenum ditelluride film is generated on a substrate through the reaction of a molybdenum source and tellurium vapor at high temperature. The method is the most effective method for preparing large-area high-crystallization-quality molybdenum ditelluride, has advantages in the aspects of size, layer number and physical property control, but the current preparation process is not mature. The biggest current problem limiting the practical application of ultra-thin two-dimensional layered materials is the acquisition of high quality wafer-level materials. The method for obtaining the large-area single-layer or multi-layer molybdenum ditelluride material by a simple and easy-to-operate and control mode has great significance and is one of the key challenges of the application.
Disclosure of Invention
The invention aims to provide a method for growing a large-area single-layer or multi-layer molybdenum ditelluride structure by secondary reaction. The method is simple to operate and good in controllability, the growth area and the number of layers of the molybdenum ditelluride are controlled by controlling the reaction temperature and the reaction time, and a large-area single-layer or multi-layer molybdenum ditelluride structure can be prepared on a substrate of 100 square centimeters.
The invention relates to a method for growing a large-area single-layer or multi-layer molybdenum ditelluride structure by secondary reaction, which comprises the following steps:
depositing a molybdenum telluride nano film on a silicon wafer, a sapphire wafer, a quartz wafer, aluminum oxide or silicon dioxide substrate with the size of 1-100 square centimeters by using an atomic layer deposition mode, wherein the deposition temperature is 100-500 ℃, and the deposition time is 10 minutes-5 hours; and then carrying out high-temperature secondary reaction on the substrate deposited with the molybdenum telluride nano film and elemental tellurium by taking inert gas or hydrogen as carrier gas, controlling the flow rate of the carrier gas to be 1-500 cubic centimeters per second, the reaction pressure to be 10-300 torr, the reaction temperature to be 600-1000 ℃, and the reaction time to be 1-10 minutes, thus obtaining a large-area single-layer or multi-layer molybdenum ditelluride structure on the substrate.
The invention has the advantages that: good controllability and simple operation, and can realize large-area preparation of molybdenum ditelluride. The single-layer or multi-layer molybdenum ditelluride structure prepared by the invention has wide application prospect in the aspects of optical materials, storage materials, catalytic materials, semiconductor photoelectric materials and the like.
Detailed Description
Example 1
Depositing a molybdenum telluride nano film on a silicon substrate with the size of 100 square centimeters by using atomic layer deposition, wherein the deposition temperature is 500 ℃, and the deposition time is 10 minutes; and then carrying out high-temperature secondary reaction on the substrate deposited with the molybdenum telluride nano film and elemental tellurium in an argon atmosphere at the reaction temperature of 1000 ℃, the reaction pressure of 80 torr and the reaction time of 1 minute to obtain a large-area single-layer molybdenum ditelluride structure.
Example 2
Depositing a molybdenum telluride nano film on a sapphire sheet substrate with the size of 66 square centimeters by using atomic layer deposition, wherein the deposition temperature is 380 ℃, and the deposition time is 5 hours; and then carrying out high-temperature secondary reaction on the substrate deposited with the molybdenum telluride nano film and elemental tellurium in an argon atmosphere, wherein the reaction temperature is 710 ℃, the reaction pressure is 170 torr, and the reaction time is 3 minutes, so that the large-area multilayer molybdenum ditelluride structure is obtained.
Example 3
Depositing a molybdenum telluride nano film on an aluminum oxide substrate with the size of 4 square centimeters by using atomic layer deposition, wherein the deposition temperature is 100 ℃, and the deposition time is 150 minutes; and then carrying out high-temperature secondary reaction on the substrate deposited with the molybdenum telluride nano film and elemental tellurium in an argon atmosphere at the reaction temperature of 600 ℃, the reaction pressure of 230 torr and the reaction time of 7 minutes to obtain the large-area multilayer molybdenum ditelluride structure.
Example 4
Firstly, depositing a molybdenum telluride nano film on a silicon dioxide substrate with the size of 25 square centimeters by using atomic layer deposition, wherein the deposition temperature is 230 ℃, and the deposition time is 30 minutes; and then carrying out high-temperature secondary reaction on the substrate deposited with the molybdenum telluride nano film and elemental tellurium in a hydrogen atmosphere, wherein the reaction temperature is 860 ℃, the reaction pressure is 50 torr, and the reaction time is 10 minutes, so that a large-area single-layer molybdenum ditelluride structure is obtained.
Claims (3)
1. A method for growing a large-area single-layer or multi-layer molybdenum ditelluride structure by secondary reaction is characterized by comprising the following steps:
firstly, molybdenum hexacarbonyl and diethyl tellurium are used as precursors, and a molybdenum telluride nano film is deposited on a substrate through atomic layer deposition; and then carrying out high-temperature secondary reaction on the substrate deposited with the molybdenum telluride nano film and elemental tellurium by taking inert gas or hydrogen as carrier gas, controlling the flow rate of the carrier gas to be 1-500 cubic centimeters per second, the reaction pressure to be 10-300 torr, the reaction temperature to be 600-1000 ℃, and the reaction time to be 10 seconds-10 minutes, thus obtaining a large-area single-layer or multi-layer molybdenum ditelluride structure on the substrate.
2. The method of claim 1, wherein the second reaction is carried out to grow a large-area single-layer or multi-layer molybdenum ditelluride structure: the substrate in the step 1 is a silicon wafer, a sapphire wafer, a quartz wafer, aluminum oxide or silicon dioxide, and the size of the substrate is 1-100 square centimeters.
3. The method of claim 1, wherein the second reaction is carried out to grow a large-area single-layer or multi-layer molybdenum ditelluride structure: the temperature of the atomic layer deposition molybdenum telluride nano film in the step 1 is 100 ℃ to 500 ℃, and the time is 10 minutes to 10 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911093705.1A CN110923663A (en) | 2019-11-11 | 2019-11-11 | Method for growing large-area single-layer or multi-layer molybdenum ditelluride structure through secondary reaction |
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| CN201911093705.1A CN110923663A (en) | 2019-11-11 | 2019-11-11 | Method for growing large-area single-layer or multi-layer molybdenum ditelluride structure through secondary reaction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113839044A (en) * | 2021-11-29 | 2021-12-24 | 广东工业大学 | Lithium-sulfur battery positive electrode, preparation method thereof and lithium-sulfur battery |
| CN114807848A (en) * | 2022-04-20 | 2022-07-29 | 南京大学 | Large-area PLD (pulsed laser deposition) preparation method of molybdenum ditelluride |
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| CN103757602A (en) * | 2014-01-13 | 2014-04-30 | 清华大学 | Method for preparing single-layer molybdenum disulfide film |
| CN105800566A (en) * | 2016-04-15 | 2016-07-27 | 中国科学院上海技术物理研究所 | Method for growing single-layer and multi-layer transition metal sulfides through alternating injection of reactants |
| CN105887015A (en) * | 2016-04-15 | 2016-08-24 | 中国科学院上海技术物理研究所 | Step-by-step gas phase method for preparing large-area single-layer tungsten disulfide and molybdenum disulfide structures |
| CN107937884A (en) * | 2017-09-19 | 2018-04-20 | 云南师范大学 | A kind of atomic layer deposition preparation method of large area molybdenum disulfide film |
| CN108389779A (en) * | 2018-02-13 | 2018-08-10 | 江南大学 | A kind of preparation method of the half-metallic telluride molybdenum based on mild hydrogen gas plasma |
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2019
- 2019-11-11 CN CN201911093705.1A patent/CN110923663A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103757602A (en) * | 2014-01-13 | 2014-04-30 | 清华大学 | Method for preparing single-layer molybdenum disulfide film |
| CN105800566A (en) * | 2016-04-15 | 2016-07-27 | 中国科学院上海技术物理研究所 | Method for growing single-layer and multi-layer transition metal sulfides through alternating injection of reactants |
| CN105887015A (en) * | 2016-04-15 | 2016-08-24 | 中国科学院上海技术物理研究所 | Step-by-step gas phase method for preparing large-area single-layer tungsten disulfide and molybdenum disulfide structures |
| CN107937884A (en) * | 2017-09-19 | 2018-04-20 | 云南师范大学 | A kind of atomic layer deposition preparation method of large area molybdenum disulfide film |
| CN108389779A (en) * | 2018-02-13 | 2018-08-10 | 江南大学 | A kind of preparation method of the half-metallic telluride molybdenum based on mild hydrogen gas plasma |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113839044A (en) * | 2021-11-29 | 2021-12-24 | 广东工业大学 | Lithium-sulfur battery positive electrode, preparation method thereof and lithium-sulfur battery |
| CN114807848A (en) * | 2022-04-20 | 2022-07-29 | 南京大学 | Large-area PLD (pulsed laser deposition) preparation method of molybdenum ditelluride |
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