CN109336181A - A kind of preparation method of two dimension Transition-metal dichalcogenide - Google Patents

A kind of preparation method of two dimension Transition-metal dichalcogenide Download PDF

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Publication number
CN109336181A
CN109336181A CN201811101185.XA CN201811101185A CN109336181A CN 109336181 A CN109336181 A CN 109336181A CN 201811101185 A CN201811101185 A CN 201811101185A CN 109336181 A CN109336181 A CN 109336181A
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preparation
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马丽颖
潘亚苹
王习习
赵乃勤
师春生
刘恩佐
何芳
沙军威
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Tianjin University
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Tianjin University
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    • 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
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
    • 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
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer

Abstract

The present invention relates to a kind of preparation methods of two-dimentional Transition-metal dichalcogenide, specifically give preparation two dimension WS2Preparation method, two-dimentional MoS2And two dimension WS2xTe2(1‑x)Preparation method, wherein two-dimentional WS2Preparation include: prepare 1g sulphur powder and 30mg WO3, sulphur powder is put into the low-temperature space of double temperature-area tubular furnaces, by WO3It is put into high-temperature region, and by Si/SiO2Substrate is tipped upside down on equipped with WO3Noah's ark on, substrate has 5-9mm at a distance from Noah's ark, is passed through Ar later, drains air；It is passed through Ar gas and H2；Low-temperature space temperature is transferred to 180-220 DEG C, high-temperature region temperature is transferred to 830-870 DEG C, growth time 3-6min.

Description

A kind of preparation method of two dimension Transition-metal dichalcogenide
Technical field
The invention belongs to the technical fields of two-dimentional Transition-metal dichalcogenide (TMDs) preparation, and in particular to arrive a kind of system For large stretch of uniform monolayers MoS having a size of 50-60 μm2、WS2And WS2xTe2(1-x)Preparation method.
Background technique
In recent years, the two chalcogenide MX of transition metal of single layer and few layer2(M=Mo, W；X=S, Se, Te) rely on Its unique, excellent optics and Electronic Performance are more and more paid close attention to by people.It is similar with the structure of graphene, TMDs X- The hexagonal lattice structure of M-X three-layer unit composition, in layer between atom by being covalently keyed, between layers by Van der Waals force Connection.Block-like TMDs is indirect band gap structure, and the TMDs of single layer and few layer is direct band gap structure, and with the number of plies It reduces, band gap is increasing, semiconductive enhancing.Therefore, the TMDs of single layer and few layer is by sizable band gap, relatively high Carrier mobility and strong photoluminescent property have a wide range of applications in semiconductor and field effect transistor field, and strong The destruction of big Quantum geometrical phase and inversion symmetry also becomes the perfect diagnostic cast of paddy electronics and spintronics Type.In addition to this, there is extremely low hydrogen to adsorb Gibbs free energy (precious metals pt is close) on the boundary of two-dimensional TM Ds, have high Electrocatalytic hydrogen evolution performance, and two-dimensional structure also provides very good model for its electro catalytic mechanism.Currently, MoS2And WS2By it The diversity of unique property and preparation method is the Typical Representative in TMDs race.
Most of two dimension transient metal sulfide is all the semiconductor property of 2H structure, and electric conductivity is bad, and unfavorable It is reacted in electrocatalytic hydrogen evolution.WTe2Belong to 1T structure under normal temperature conditions, there is metallicity, electric conductivity is excellent. WS2xTe2(1-x)The adjustable band gap width of ternary alloy three-partalloy, WS2Band gap width be 1.9ev, WTe2Band gap width be about 0ev, WS2xTe2(1-x)Band gap width between 0-1.9ev, realize from semiconductor to Metal Phase Transition.
So far, the TMDs preparation method of common single layer and few layer has mechanical and liquid stripping method, molecular beam epitaxy Method and chemical vapour deposition technique (CVD) etc..Currently, main stream approach is chemical vapor deposition method, easy to operate, the material of preparation Size, thickness are controllable, low cost, are suitble to large scale preparation and study two-dimensional TMDs.But due to the unique property of TMDs, Still there is great challenge for controllable preparation large scale, uniform, single layer TMDs.
Summary of the invention
In view of the deficiencies of the prior art, the technical issues of present invention intends to solve is: providing and a kind of prepares single layer and few layer MoS2, WS2 and WS2xTe2(1-x)Method, being capable of controlled dimensions (WS2Reach 50-60 μm, MoS2Reach 120 μm, WS2xTe2(1-x) Reach 50-60 μm), thickness (single layer) and uniformity.The present invention using CVD method, operating method is simple, it is low in cost, Program is controllable.By regulating and controlling temperature, time, throughput and the pressure of CVD precursors, can be obtained required single layer and The WS of few layer2、MoS2And WS2xTe2(1-x).Technical solution is as follows:
(1) a kind of two dimension WS2Preparation method, including the following steps:
1) prepare the sulphur powder of 1g and the WO of 30mg3, sulphur powder is put into the low-temperature space of double temperature-area tubular furnaces, by WO3It is put into high temperature Area, and by Si/SiO2Substrate is tipped upside down on equipped with WO3Noah's ark on, substrate has 5-9mm at a distance from Noah's ark, be passed through Ar later, arrange Walk air；
2) Ar gas and H are passed through2；
3) low-temperature space temperature is transferred to 180-220 DEG C, high-temperature region temperature is transferred to 830-870 DEG C, growth time 3-6min.
(2) a kind of two dimension MoS2Preparation method, including the following steps:
1) prepare sulphur powder and MoO according to the quality proportioning of 1:0.002-0.0043, sulphur powder is put into the low of double temperature-area tubular furnaces Warm area, MoO3It is put into high-temperature region, Si/SiO2Matrix, which tips upside down on, contains MoO3Noah's ark on, substrate has 5-9mm at a distance from Noah's ark, it After be passed through Ar, drain air；
2) Ar gas and H are passed through2；
3) low-temperature space temperature is transferred to 180-220 DEG C, high-temperature region temperature is transferred to 780-820 DEG C, growth time 3-6min.
(3) a kind of two dimension WS2xTe2(1-x)Preparation method, including the following steps:
1) the tellurium powder of 1g is put into the low-temperature space of double temperature-area tubular furnaces, it will be according to the two-dimentional WS prepared by (1)2It is put into tubular type The high-temperature region of furnace, is passed through Ar later, drains air；
2) Ar gas and H are passed through2；
3) temperature switch is opened, low-temperature space temperature is transferred to 400-500 DEG C, high-temperature region temperature is transferred to 600-750 DEG C, growth Time 3-4h.
Compared with prior art, the two-dimentional Transition-metal dichalcogenide (WS that the present invention obtains2、MoS2、 WS2xTe2(1-x)) with a thickness of single layer, it is evenly distributed, size is larger, and quality is higher, and method is simple, and it is low in cost, reduce to ring The harm in border.
Detailed description of the invention
Fig. 1 is two-dimentional WS prepared by the embodiment of the present invention 12Low power light microscopic figure, can be seen that from map, it is prepared Product is evenly distributed with a thickness of single layer, and size is larger, and quality is higher；
Fig. 2 is two-dimentional WS prepared by the embodiment of the present invention 12High power light microscopic figure, can be seen that from map, it is prepared Product is evenly distributed with a thickness of single layer, and size is larger, and quality is higher；
Fig. 3 is two-dimentional WS prepared by the embodiment of the present invention 12Raman figure, it was found from two frequency peak to peak values of Raman figure The two-dimentional WS2 of generation is in single layer；
Fig. 4 is two-dimentional MoS prepared by the embodiment of the present invention 22Low power light microscopic figure, can be seen that from map, it is prepared Product with a thickness of single layer, be evenly distributed, size is larger, and quality is higher；
Fig. 5 is two-dimentional MoS prepared by the embodiment of the present invention 22High power light microscopic figure, can be seen that from map, it is prepared Product with a thickness of single layer, be evenly distributed, size is larger, and quality is higher；
Fig. 6 is two-dimentional MoS prepared by the embodiment of the present invention 22Raman figure, can from two frequency peak to peak values of Raman figure Know the two-dimentional MoS of generation2In single layer；
Fig. 7 is two-dimentional WS prepared by the embodiment of the present invention 32xTe2(1-x)Low power light microscopic figure, can be seen that from map, Prepared product is evenly distributed with a thickness of single layer, and size is larger, and quality is higher；
The present invention does not address place and is suitable for the prior art.
The specific embodiment of preparation method of the present invention is given below.Preparation that these embodiments are only used for that the present invention will be described in detail Method is not intended to limit the protection scope of the claim of this application.
Embodiment 1
Size is prepared at 50 μm or more, is had with a thickness of single layer, the two-dimentional WS being evenly distributed2。
(1) sulphur powder of 1g is put into the low-temperature space of double temperature-area tubular furnaces, the WO of 30mg3It is put into the high-temperature region of tube furnace, Si/ SiO2Substrate, which tips upside down on, contains WO3Noah's ark on, substrate has 7mm at a distance from Noah's ark, later lead to 500sccm Ar gas, keep 15min drains air；
(2) after, the Ar gas of 80sccm and the H of 10sccm are passed through2, condition of normal pressure；
(3) temperature switch is opened, low-temperature space temperature is transferred to 200 DEG C, high-temperature region temperature is transferred to 850 DEG C, and growth time is protected Hold 3min；
(4) by 3) obtained in WS2Shifted (spin coating PMMA, etching Si/SiO2Substrate, transfer WS2, drying, acetone Remove PMMA), it is characterized.
Embodiment 2
Size is prepared at 120 μm or more, is had with a thickness of single layer, the two-dimentional MoS being evenly distributed2。
(1) sulphur powder of 1g is put into the low-temperature space of double temperature-area tubular furnaces, the MoO of 3mg3It is put into the high-temperature region of tube furnace, Si/ SiO2Matrix, which tips upside down on, contains MoO3Noah's ark on, substrate has 7mm at a distance from Noah's ark, later lead to 500sccm Ar gas, keep 15min drains air；
(2) after, the Ar gas of 80sccm and the H of 10sccm are passed through2；
(3) temperature switch is opened, low-temperature space temperature is transferred to 200 DEG C, high-temperature region temperature is transferred to 800 DEG C, and growth time is protected Hold 3min；
(4) by 3) obtained in MoO3Shifted (spin coating PMMA, etching Si/SiO2Substrate, transfer MoO3, drying, third Ketone removes PMMA), it is characterized.
Embodiment 3
50 μm of preparation or more has with a thickness of single layer, the two-dimentional WS being evenly distributed2xTe2(1-x)。
(1) the tellurium powder of 1g is put into the low-temperature space of double temperature-area tubular furnaces, by WS manufactured in embodiment 12It is put into tube furnace High-temperature region, later lead to 500sccm Ar gas, keep 15min, drain air；
(2) after, the Ar gas of 10sccm and the H of 4sccm are passed through2；
(3) temperature switch is opened, low-temperature space temperature is transferred to 460 DEG C, high-temperature region temperature is transferred to 650 DEG C, growth time 4h；
(4) by WS obtained in (3)2xTe2(1-x)It is shifted, is characterized.

Claims (3)

1. a kind of two dimension WS2Preparation method, including the following steps:
1) prepare the sulphur powder of 1g and the WO of 30mg3, sulphur powder is put into the low-temperature space of double temperature-area tubular furnaces, by WO3High-temperature region is put into, And by Si/SiO2Substrate is tipped upside down on equipped with WO3Noah's ark on, substrate has 5-9mm at a distance from Noah's ark, is passed through Ar later, drains sky Gas.
2) Ar gas and H are passed through2；
3) low-temperature space temperature is transferred to 180-220 DEG C, high-temperature region temperature is transferred to 830-870 DEG C, growth time 3-6min.
2. a kind of two dimension MoS2Preparation method, including the following steps:
1) prepare sulphur powder and MoO according to the quality proportioning of 1:0.002-0.0043, sulphur powder is put into the low-temperature space of double temperature-area tubular furnaces, MoO3It is put into high-temperature region, Si/SiO2Matrix, which tips upside down on, contains MoO3Noah's ark on, substrate has 5-9mm, Zhi Houtong at a distance from Noah's ark Enter Ar, drains air；
2) Ar gas and H are passed through2；
3) low-temperature space temperature is transferred to 180-220 DEG C, high-temperature region temperature is transferred to 780-820 DEG C, growth time 3-6min.
3. a kind of two dimension WS2xTe2(1-x)Preparation method, including the following steps:
1) the tellurium powder of 1g is put into the low-temperature space of double temperature-area tubular furnaces, by two-dimentional WS prepared according to claim 12It is put into pipe The high-temperature region of formula furnace, is passed through Ar later, drains air；
2) Ar gas and H are passed through2；
3) temperature switch is opened, low-temperature space temperature is transferred to 400-500 DEG C, high-temperature region temperature is transferred to 600-750 DEG C, growth time 3-4h。
CN201811101185.XA 2018-09-20 2018-09-20 A kind of preparation method of two dimension Transition-metal dichalcogenide Pending CN109336181A (en)

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CN110093591A (en) * 2019-04-09 2019-08-06 南京邮电大学 The preparation method of two-dimentional Transition-metal dichalcogenide material
CN110257906A (en) * 2019-07-23 2019-09-20 西北工业大学 A kind of two dimension Transition-metal dichalcogenide crystal and its preparation method and application
CN110344023A (en) * 2019-08-08 2019-10-18 中北大学 A kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate2The preparation method of film
CN110563040A (en) * 2019-09-27 2019-12-13 天津大学 Preparation method of tungsten disulfide nanosheet for electrocatalytic hydrogen evolution
CN112079386A (en) * 2020-09-16 2020-12-15 长春理工大学 MoS2Preparation method for regulating and controlling S vacancy defects of two-dimensional material
CN112663021A (en) * 2020-11-03 2021-04-16 杭州电子科技大学 Preparation method of two-dimensional molybdenum-tungsten-sulfur vertical heterostructure
CN114014363A (en) * 2021-12-03 2022-02-08 河北大学 Two-dimensional WX2Material and method for the production thereof

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Publication number Priority date Publication date Assignee Title
CN110093591A (en) * 2019-04-09 2019-08-06 南京邮电大学 The preparation method of two-dimentional Transition-metal dichalcogenide material
CN110257906A (en) * 2019-07-23 2019-09-20 西北工业大学 A kind of two dimension Transition-metal dichalcogenide crystal and its preparation method and application
CN110257906B (en) * 2019-07-23 2021-07-27 西北工业大学 Two-dimensional transition metal chalcogenide crystal and preparation method and application thereof
CN110344023A (en) * 2019-08-08 2019-10-18 中北大学 A kind of single layer WS of low-temp low-pressure vapor deposition high coverage rate2The preparation method of film
CN110344023B (en) * 2019-08-08 2021-09-07 中北大学 Low-temperature low-pressure vapor deposition high-coverage single-layer WS2Method for producing thin film
CN110563040A (en) * 2019-09-27 2019-12-13 天津大学 Preparation method of tungsten disulfide nanosheet for electrocatalytic hydrogen evolution
CN112079386A (en) * 2020-09-16 2020-12-15 长春理工大学 MoS2Preparation method for regulating and controlling S vacancy defects of two-dimensional material
CN112663021A (en) * 2020-11-03 2021-04-16 杭州电子科技大学 Preparation method of two-dimensional molybdenum-tungsten-sulfur vertical heterostructure
CN114014363A (en) * 2021-12-03 2022-02-08 河北大学 Two-dimensional WX2Material and method for the production thereof

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