CN110863189A - Method for growing single-layer telluride doped structure by pulse type injection of reactant - Google Patents
Method for growing single-layer telluride doped structure by pulse type injection of reactant Download PDFInfo
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- CN110863189A CN110863189A CN201911093527.2A CN201911093527A CN110863189A CN 110863189 A CN110863189 A CN 110863189A CN 201911093527 A CN201911093527 A CN 201911093527A CN 110863189 A CN110863189 A CN 110863189A
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- telluride
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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
- C23C16/45557—Pulsed pressure or control pressure
Abstract
The invention discloses a method for growing a single-layer telluride doped structure by pulse type injection of reactants. The method simultaneously injects a plurality of transition metal organic matters and diethyl tellurium or injects molybdenum hexacarbonyl and a plurality of sulfur group elements to control the flow rate of carrier gas to control the doping amount of telluride, and controls the reaction temperature and the reaction time to control the area and the layer number of the growth of the telluride, thereby obtaining the molybdenum ditelluride with a high-quality doping structure. The invention has the advantages that: the growth condition is accurate and controllable, the operation is simple and convenient, and the stable molybdenum ditelluride with a single-layer doping structure can be prepared. The molybdenum ditelluride with the single-layer doped structure prepared by the invention has wide application prospect in the fields of nano electronic devices, lubricating materials, photocatalysis and the like.
Description
Technical Field
The invention belongs to the field of material preparation, relates to a nano material preparation technology, and particularly relates to a method for growing a single-layer telluride doped structure by pulse injection of reactants.
Background
Since Novoseov and Geim and co-workers in 2004 successfully used adhesive tapes to strip graphene from graphite, research on two-dimensional materials has entered a period of rapid development, and at the same time, graphene and graphene-like materials further enrich the family of two-dimensional materials, such as two-dimensional transition metal chalcogenides, which have excellent physicochemical properties and unique thermoelectric, conductive, superconducting, optical, and photovoltaic properties, making them have a wide application prospect in the fields of optical materials, memory materials, catalytic materials, semiconductor photoelectric materials, and the like.
Although two-dimensional nanomaterials show attractive prospects, the bottleneck that restricts the development thereof is how to prepare high-quality 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 former 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 latter is the most efficient method for preparing large-area high-crystalline-quality molybdenum ditelluride, and has advantages in the aspects of size, layer number and physical property control, but the current preparation process is still immature. Two-dimensional materials are susceptible to doping with some other molecule, atom or ion between layers of the two-dimensional material due to weak van der waals forces between layers. Taking transition metal sulfide as an example, with the change of the species or concentration of interlayer intercalation components, the intrinsic electronic structure of the transition metal sulfide can be effectively regulated and controlled, and various peculiar physical or chemical phenomena can be caused, such as charge density waves, anisotropic transport performance, even superconductivity and other various electronic behaviors. Doping is an effective method for regulating and controlling the physical and chemical properties of a two-dimensional material, and a single-layer telluride doped structure is obtained in a simple and easy-to-operate and control mode, so that the method has great significance and is one of the key challenges of application.
Disclosure of Invention
It is an object of the present invention to provide a method of growing a single layer telluride doped structure. The method is simple and convenient to operate and good in controllability, and by injecting the reactants into the reaction cavity in a pulse mode, the dosage of the reactants, the reaction temperature and the pulse time are accurately controlled, so that the reactants enter the cavity in the pulse mode to carry out deposition reaction, the doping atomic weight, the growth area and the number of layers of the molybdenum ditelluride are controlled, and the telluride with a stable single-layer doping structure is prepared.
The invention relates to a method for growing a single-layer telluride doping structure by pulse type injection of reactants, which comprises the following steps:
firstly, a clean substrate with the area of 1-100 square centimeters, such as a silicon, sapphire sheet, quartz sheet or a substrate with an aluminum oxide and silicon dioxide film growing on the surface is placed in a reaction cavity, and the reaction pressure is controlled to be 10-300 torr; and injecting various transition metal organic matters and diethyl tellurium or injecting molybdenum hexacarbonyl and various chalcogen elements in a pulse mode 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, controlling the pulse time of injecting different reactants to be 1-5 minutes, performing pulse injection for 1-800 times in a total cycle, controlling the reaction temperature to be 600-900 ℃, and obtaining the telluride with a single-layer doping structure on the substrate.
The transition metal organic matter is molybdenum hexacarbonyl or tungsten hexacarbonyl.
The chalcogen is diethyl sulfur, diethyl tellurium or diethyl diselenide.
The invention has the advantages that: the growth condition is accurate and controllable, the operation is simple and convenient, and the preparation of doped structure telluride can be realized. Has wide application prospect in the fields of nano electronic devices, lubricating materials, photocatalysis, and the like.
Detailed Description
Example 1
Placing a clean silicon substrate of 100 square centimeters in a deposition reaction cavity, and controlling the reaction pressure at 300 torr and the reaction temperature at 900 ℃; pulse-type injection of molybdenum hexacarbonyl, tungsten hexacarbonyl and diethyl tellurium into a cavity by carrier gas, setting the flow rate of the carrier gas to be 500 cubic centimeters per second, the pulse injection time of molybdenum hexacarbonyl to be 1 minute, the pulse injection time of tungsten hexacarbonyl to be 7 seconds, the pulse injection time of diethyl tellurium to be 3 minutes, and injecting 200 cycles in total to obtain a single-layer Mo by deposition0.9W0.1Te2。
Example 2
Placing a clean silicon substrate of 6 square centimeters in a deposition reaction cavity, and controlling the reaction pressure at 40 torr and the reaction temperature at 600 ℃; pulse-type injection of molybdenum hexacarbonyl, tungsten hexacarbonyl and diethyl tellurium into the cavity by carrier gas, setting carrier gas flow rate at 60 cubic centimeter/second, pulse injection time of molybdenum hexacarbonyl at 30 seconds, pulse injection time of tungsten hexacarbonyl at 10 seconds, pulse injection time of diethyl tellurium at 2 minutes, co-injectingEntering 400 cycles, depositing to obtain a single Mo layer0.8W0.2Te2。
Example 3
Placing a clean silicon substrate with the thickness of 54 square centimeters in a deposition reaction cavity, controlling the reaction pressure at 230 torr and the reaction temperature at 710 ℃; pulse-type injection of molybdenum hexacarbonyl, diethyl sulfur and diethyl tellurium into a cavity by carrier gas, setting the flow rate of the carrier gas to be 80 cubic centimeters per second, the pulse injection time of the molybdenum hexacarbonyl to be 1 minute, the pulse injection time of the diethyl sulfur to be 30 seconds and the pulse injection time of the diethyl tellurium to be 4 minutes, injecting the mixture for 800 cycles in total, and depositing to obtain single-layer MoS0.4Te1.6。
Example 4
Placing a clean silicon substrate with 27 square centimeters in a deposition reaction cavity, and controlling the reaction pressure at 170 torr and the reaction temperature at 760 ℃; pulse-type injection of molybdenum hexacarbonyl, diethyl diselenide and diethyl tellurium into the cavity by carrier gas, setting the flow rate of the carrier gas to be 420 cubic centimeters per second, the pulse injection time of the molybdenum hexacarbonyl to be 2 minutes, the pulse injection time of the diethyl diselenide to be 1 minute, the pulse injection time of the diethyl tellurium to be 5 minutes, co-injection of 340 cycles, deposition to obtain single-layer MoSe0.3Te1.6。
Claims (3)
1. A method for growing a single-layer telluride doped structure by injecting reactants in a pulse mode is characterized by comprising the following steps:
firstly, a clean substrate with the area of 1-100 square centimeters, such as a silicon, sapphire sheet, quartz sheet or a substrate with an aluminum oxide and silicon dioxide film growing on the surface is placed in a reaction cavity, and the reaction pressure is controlled to be 10-300 torr; and injecting various transition metal organic matters and diethyl tellurium or injecting molybdenum hexacarbonyl and various chalcogen elements in a pulse mode 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, controlling the pulse time of injecting different reactants to be 1-5 minutes, performing pulse injection for 1-800 times in a total cycle, controlling the reaction temperature to be 600-900 ℃, and obtaining the telluride with a single-layer doping structure on the substrate.
2. The method of claim 1, wherein the step of growing the single-layer telluride doped structure comprises the steps of: the transition metal organic matter is molybdenum hexacarbonyl or tungsten hexacarbonyl.
3. The method of claim 1, wherein the step of growing the single-layer telluride doped structure comprises the steps of: the chalcogen is diethyl sulfur, diethyl tellurium or diethyl diselenide.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112342522A (en) * | 2020-09-15 | 2021-02-09 | 中国科学院上海技术物理研究所 | Method for preparing large-area single-layer and multi-layer gallium telluride materials by alternative reactants |
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CN103124806A (en) * | 2010-09-29 | 2013-05-29 | 东京毅力科创株式会社 | Method for forming Ge-Sb-Te film and storage medium |
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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 |
WO2018065321A1 (en) * | 2016-10-04 | 2018-04-12 | Kobus Sas | Method for injecting chemical species in the gas phase in plasma-pulsed form |
CN107923039A (en) * | 2015-05-27 | 2018-04-17 | Asm Ip 控股有限公司 | Synthesis and purposes for the precursor containing molybdenum or the ALD of W film |
US20180216232A1 (en) * | 2015-09-15 | 2018-08-02 | Ultratech, Inc. | Laser-Assisted Atomic Layer Deposition of 2D Metal Chalcogenide Films |
CN109423617A (en) * | 2017-08-30 | 2019-03-05 | Asm Ip控股有限公司 | Deposited on the dielectric surface of substrate by cyclic deposition process molybdenum film method and associated semiconductor device structure |
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- 2019-11-11 CN CN201911093527.2A patent/CN110863189A/en active Pending
Patent Citations (7)
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CN103124806A (en) * | 2010-09-29 | 2013-05-29 | 东京毅力科创株式会社 | Method for forming Ge-Sb-Te film and storage medium |
CN107923039A (en) * | 2015-05-27 | 2018-04-17 | Asm Ip 控股有限公司 | Synthesis and purposes for the precursor containing molybdenum or the ALD of W film |
US20180216232A1 (en) * | 2015-09-15 | 2018-08-02 | Ultratech, Inc. | Laser-Assisted Atomic Layer Deposition of 2D Metal Chalcogenide Films |
CN105734528A (en) * | 2016-03-09 | 2016-07-06 | 无锡盈芯半导体科技有限公司 | Growth method for layered molybdenum disulfide films on basis of pulse airflow method |
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 |
WO2018065321A1 (en) * | 2016-10-04 | 2018-04-12 | Kobus Sas | Method for injecting chemical species in the gas phase in plasma-pulsed form |
CN109423617A (en) * | 2017-08-30 | 2019-03-05 | Asm Ip控股有限公司 | Deposited on the dielectric surface of substrate by cyclic deposition process molybdenum film method and associated semiconductor device structure |
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CN112342522A (en) * | 2020-09-15 | 2021-02-09 | 中国科学院上海技术物理研究所 | Method for preparing large-area single-layer and multi-layer gallium telluride materials by alternative reactants |
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