CN114574955B - Preparation method of catalyst double-assisted two-dimensional transition metal chalcogenide film - Google Patents

Preparation method of catalyst double-assisted two-dimensional transition metal chalcogenide film Download PDF

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CN114574955B
CN114574955B CN202210212260.XA CN202210212260A CN114574955B CN 114574955 B CN114574955 B CN 114574955B CN 202210212260 A CN202210212260 A CN 202210212260A CN 114574955 B CN114574955 B CN 114574955B
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quartz boat
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CN114574955A (en
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唐宁
樊腾
刘星辰
张仕雄
王奋陶
孙真昊
姜稼阳
李国平
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    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C—CHEMISTRY; METALLURGY
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    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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    • C—CHEMISTRY; METALLURGY
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    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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Abstract

The invention discloses a preparation method of a catalyst double-auxiliary two-dimensional transition metal chalcogenide film (TMDs). In the method, a quartz boat with an opening at one end and a closed end is adopted to hold a metal source in the process of preparing the TMDS film by using a chemical vapor deposition method, the growth surface of a substrate is downwards buckled at the closed end of the quartz boat to form a semi-closed structure, and a carrier gas carries the source to form vortex below the substrate, so that the source partial pressure of the growth surface of the substrate is larger and more uniform, and the problems of film discontinuity and uneven crystal quality are avoided; meanwhile, a halide catalyst double-auxiliary method is adopted, and catalysts are added into the metal source and the growing surface of the substrate at the same time, so that the source partial pressure is further improved, and the growth time is shortened; and the controllable growth of TMDS films with different layers is realized by changing the concentration of the catalyst solution which is spin-coated on the surface of the substrate. The method for preparing the TMDS film has the advantages of controllable film thickness, complete crystal form and high repeatability.

Description

Preparation method of catalyst double-assisted two-dimensional transition metal chalcogenide film
Technical Field
The invention belongs to the technical field of preparation of two-dimensional materials, and particularly relates to a preparation method of a two-dimensional transition metal chalcogenide (TMDS) film.
Background
Two-dimensional transition metal chalcogenide MX 2 The single-layer TMDS film has the characteristic of valence band splitting and large valley polarizability, is widely researched in the aspects of spintronics and valley electronics, and is considered as one of key materials in the later molar era. The wide application of two-dimensional layered transition metal chalcogenide (TMDCs) materials requires the development of reliable preparation methods. Researchers have explored a variety of methods to obtain high quality single layer TMDs materials, including mechanical lift-off, molecular beam epitaxy, physical vapor deposition, and Chemical Vapor Deposition (CVD). Among these methods, CVD has a great potential for reproducibly producing high-quality large-area single-layer single crystals.
Although significant progress has been made in the CVD process for producing TMDs, it still faces many problems such as uncontrollable film thickness, poor reproducibility, non-uniform source partial pressure, non-uniform crystal quality of the thin film, etc. The synthesis of large-area, continuous, high-quality, layer-number-controllable TMDs films by CVD methods remains challenging.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a halide double-auxiliary two-dimensional transition metal chalcogenide film, which utilizes the double-auxiliary action of airflow vortex and catalyst to realize the large-area, continuous, high-quality and layer-number-controllable two-dimensional transition metal chalcogenide film.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a preparation method of two-dimensional transition metal chalcogenide (TMDS) film, prepare TMDS film through the chemical vapor deposition method, characterized by that, adopt and hold the metal source in the quartz boat that one end opening end is closed in the horizontal direction, buckle the growth surface of the substrate on the closed end of quartz boat downward, form a kind of semi-closed structure, then put into tube furnace; in the preparation process, the carrier gas carries the source to form vortex below the substrate, so that the source partial pressure of the surface of the substrate is increased, and the problem of uneven source space distribution is effectively avoided; meanwhile, a catalyst double-auxiliary method is adopted, and a catalyst is added in a metal source and on the growth surface of the substrate.
The method grows large-area single-layer TMDs film, and solves the problems of small size and no film formation of TMDs single crystal prepared by chemical vapor deposition; the controllable growth of TMDS films with different layers is realized by adding catalysts with different concentrations to the growth surface of the substrate.
Further, the invention can adopt a dual-temperature-zone tube furnace to realize CVD, the dual-temperature-zone tube furnace is provided with an A temperature zone positioned at the upstream of the carrier gas and a B temperature zone positioned at the downstream of the carrier gas, and the method for preparing the TMDS film comprises the following steps:
a, placing a nonmetal source in a common crucible in the center of an A temperature zone of a double-temperature-zone tube furnace;
b, mixing a metal source and a catalyst, and placing the mixture in a quartz boat with an opening at one end and a closed end;
c, adding a catalyst on the growth surface of the substrate;
step d, buckling the growth surface of the substrate downwards at the closed end of the quartz boat to form a semi-closed structure, and placing the quartz boat at the center of a temperature zone B of the dual-temperature-zone tube furnace, wherein the open end is the upstream of the carrier gas;
e, repeating the steps of vacuumizing and carrier gas introducing for multiple times, removing air in the tubular furnace, and then continuously introducing the carrier gas;
f, heating the temperature zone A and the temperature zone B to the required temperature and preserving the temperature for a certain time;
and g, after the heat preservation is finished, taking out the substrate after the tubular furnace is cooled to the room temperature, and obtaining the two-dimensional TMDS film on the growth surface of the substrate.
In the above method, the non-metal source may be selected from any one or more of S, Se, Te; the metal source is selected from MoO 3 、WO 3 Any one or more of them.
Preferably, in the step b, the catalyst is halide selected from any one or more of NaCl, KCl, NaBr, KBr, NaI and KI.
Preferably, in the step b, the method for mixing the metal source and the catalyst comprises mixing the solid metal source and the solid catalyst and then grinding, or soaking the solid metal source in a solution containing the catalyst and then drying to remove the solvent; wherein the mass ratio of the metal source to the halide catalyst is 1 (0.3-3).
Preferably, in the step b, the quartz boat with one open end and one closed end has a trapezoidal longitudinal section, the upper part of the quartz boat is wide, the lower part of the quartz boat is narrow, the upper side of the trapezoid is 2-4 cm long, the lower side of the trapezoid is 1-3 cm long, and the height of the trapezoid is 1-3 cm.
Preferably, in the step c, the substrate may be a metal substrate, a Si substrate, or a substrate having SiO 2 A Si substrate, a sapphire substrate, a GaN substrate, an AlN substrate, an InN substrate, an AlGaN substrate, an InGaN substrate, or the like of the layer.
Preferably, in the step c, the substrate has a rectangular shape with a length of 2 to 5cm and a width of 1 to 3 cm.
Preferably, in the step c, the substrate is cleaned and then coated with the catalyst, and the substrate is cleaned by sequentially soaking the substrate in acetone, absolute ethyl alcohol and deionized water, performing ultrasonic treatment for 5min, and then drying the substrate by blowing or drying.
Preferably, in the step c, the method for adding the catalyst to the growth surface of the clean substrate comprises the steps of spin-coating a certain amount of solution in which the catalyst is dissolved on the growth surface of the substrate, and then blow-drying or drying;
preferably, in the step c, the catalyst is dissolved in a solvent to a concentration of 0.1 to 1mmol/L, and then applied to the growth surface of the substrate. The solvent is preferably deionized water or absolute ethyl alcohol, and the concentration of the catalyst solution is in direct proportion to the number of layers of the final TMDS film.
Preferably, in the step d, when the growth surface of the substrate is buckled downwards at the closed end of the quartz boat, a gap cannot be left between the substrate and the side wall to form a semi-closed structure, so that the airflow forms a vortex below the substrate, and the source partial pressure is improved.
Preferably, the metal source is located 1-3 cm upstream of the substrate.
Preferably, in step e, the carrier gas is an inert gas or a mixture of an inert gas and hydrogen, wherein the inert gas is preferably argon or nitrogen.
Further preferably, the mixing ratio of the inert gas and the hydrogen is any ratio; in this case, hydrogen can be introduced in a pulsed manner into the tube furnace.
Preferably, in the step f, the temperature of the temperature zone A is increased to 150-300 ℃ at the heating rate of 10-30 ℃/min, the temperature of the temperature zone B is increased to 600-900 ℃ at the heating rate of 10-30 ℃/min, and the temperature is kept for 5-20 min.
The preparation method of the two-dimensional transition metal chalcogenide (TMDS) film has the following advantages:
1. when the two-dimensional transition metal chalcogenide film is prepared by chemical vapor deposition, the quartz boat with an opening at one end and a closed end is adopted to contain the metal source, the growth surface of the substrate is downwards buckled at the closed end of the quartz boat, the substrate, three side walls and one bottom surface of the quartz boat form a semi-closed structure, the carrier gas carries the source to flow in from the open end of the quartz boat, the carrier gas is not blocked and the airflow is smoother, and a vortex is formed below the substrate, so that the source partial pressure of the growth surface of the substrate is larger and more uniform, the problem of discontinuous film caused by insufficient source partial pressure is avoided, and the problem of non-uniform film crystal quality caused by non-uniform source space distribution is also avoided;
2. the invention adopts a catalyst double-auxiliary method, and simultaneously adds the catalyst in the metal source and the growing surface of the substrate to obtain the TMDS film with large area and controllable layer number. The catalyst is added into the metal source, so that the sublimation temperature of the metal source can be reduced, the sublimation time of the metal source is shortened, the constant large partial pressure of the metal source is kept in a short time instead of the constant small partial pressure, the growth time is shortened, the source partial pressure is further improved, and the problem of discontinuous film caused by insufficient source partial pressure is solved; the controllable growth of TMDS films with different layers is realized by changing the concentration of the catalyst solution which is spin-coated on the surface of the substrate. Compared with the method for growing the single-layer TMDS film by only adding the catalyst into the metal source, the method can realize the layer number control of the TMDS film, and has the advantages of simple and convenient operation, low cost and good repeatability.
Drawings
FIG. 1 is a schematic view of a quartz boat with an open end and a closed end, a metal source and a substrate.
FIG. 2 is a schematic diagram of the arrangement positions of the temperature region A and the temperature region B of the dual-temperature-region tube furnace and the non-metal source and the metal source.
FIG. 3 shows a single-layer MoS obtained in example 1 of the present invention 2 Optical microscopy of thin films.
FIG. 4 shows a single-layer MoS obtained in example 1 of the present invention 2 Raman spectrum of the film.
FIG. 5 shows a three-layered MoS obtained in example 2 of the present invention 2 Optical microscopy of thin films.
FIG. 6 shows a three-layered MoS obtained in example 2 of the present invention 2 Raman spectrum of the film.
FIG. 7 shows a five-layer MoS obtained in example 3 of the present invention 2 Optical microscopy of thin films.
FIG. 8 shows a five-layer MoS obtained in example 3 of the present invention 2 Raman spectrum of the film.
Detailed Description
Example 1
Preparation of Single-layer MoS 2 The film, see fig. 2, is embodied as follows:
step a, weighing 200mg of sulfur powder in a common crucible, and placing the crucible in the center of an A temperature zone of a double-temperature-zone tube furnace;
step b. dissolve 5mg solid NaCl in 1mL deionized water, 10mg MoO 3 Pouring the powder into the NaCl solution, drying, and placing into a quartz boat (shown in figure 1) with one open end and one closed end, wherein the distance between the quartz boat and the side wall of the closed end is 2 cm;
step c. on clean SiO 2 SiO of/Si substrate 2 Spin coating 100 μ L NaCl solution with concentration of 0.3mmol/L, and blow-drying with nitrogen gun;
step d, SiO of the substrate 2 Covering the closed end of a quartz boat with an opening at one end and a closed end downwards to form a semi-closed structure, and placing the quartz boat in the center of a temperature zone B of the dual-temperature-zone tube furnace, wherein the opening end is the upstream of carrier gas;
repeating the step e, vacuumizing for 3-5 times,General formula (N) 2 Step (3) removing air in the tube furnace, and then continuously introducing 50-300 sccm of N 2 ；
F, raising the temperature of the temperature zone A to 200 ℃ at the heating rate of 10 ℃/min, raising the temperature of the temperature zone B to 600 ℃ at the heating rate of 30 ℃/min, and preserving the heat for 10 min;
and g, after the heat preservation is finished, taking out the substrate after the tubular furnace is cooled to the room temperature, and obtaining the two-dimensional TMDS film.
Example 2
Preparation of three-layer MoS 2 The membrane, in comparison with example 1, differs in that in step c the concentration of the NaCl solution is 0.5 mmol/L.
Example 3
Preparation of five-layer MoS 2 The membrane, in comparison with example 1, differs in that in step c the concentration of the NaCl solution is 0.8 mmol/L.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application belong to the protection scope of the claims of the present invention. The invention has not been described in detail in order to avoid obscuring the invention.

Claims (8)

1. A preparation method of two-dimensional transition metal chalcogenide film, prepare the said film through the chemical vapor deposition method, characterized by that, add catalyst in the metal source and substrate growth surface, adopt the quartz boat that one end opening is closed in the horizontal direction, hold the metal source, buckle the growth surface of the substrate on the closed end of quartz boat downward, form the semi-enclosed structure, then put the quartz boat into the tubular furnace of double temperature zone to carry on the chemical vapor deposition; the longitudinal section of the quartz boat is trapezoidal, and the upper part of the quartz boat is wide and the lower part of the quartz boat is narrow; the double-temperature-zone tube furnace is provided with an A temperature zone located at the upstream of carrier gas and a B temperature zone located at the downstream of the carrier gas, and the preparation method comprises the following steps:
a) placing a nonmetal source in a crucible in the center of an A temperature zone of a double-temperature-zone tubular furnace;
b) mixing a metal source and a catalyst, and then placing the mixture in a quartz boat with an opening at one end and a closed end;
c) adding a catalyst on the growth surface of the substrate, namely spin-coating a solution dissolved with the catalyst on the growth surface of the substrate, blow-drying or drying, and adjusting the layer number of the two-dimensional transition metal chalcogenide film by adjusting the concentration of the catalyst solution;
d) buckling the growth surface of the substrate downwards at the closed end of the quartz boat to form a semi-closed structure, and placing the quartz boat at the center of a temperature zone B of the dual-temperature-zone tube furnace, wherein the open end is the upstream of the carrier gas;
e) repeating the steps of vacuumizing and introducing carrier gas for multiple times, removing air in the tubular furnace, and continuously introducing the carrier gas;
f) heating the temperature zone A and the temperature zone B to the required temperature and preserving the temperature for a certain time;
g) and after the heat preservation is finished, taking out the substrate after the tube furnace is cooled to the room temperature, and obtaining the two-dimensional transition metal chalcogenide film on the growth surface of the substrate.
2. The method according to claim 1, wherein the non-metal source is selected from any one or more of S, Se, Te; the metal source is selected from MoO 3 、WO 3 Any one or more of them.
3. The method of claim 1, wherein the catalyst is a halide selected from any one or more of NaCl, KCl, NaBr, KBr, NaI, and KI.
4. The preparation method according to claim 3, wherein in the step b), the solid metal source and the solid catalyst are mixed and then ground, or the solid metal source is soaked in a solution dissolved with the catalyst and then dried to remove the solvent, so as to obtain a mixture of the metal source and the catalyst, wherein the mass ratio of the metal source to the catalyst is 1 (0.3-3).
5. The method of claim 1, wherein the quartz boat has a trapezoidal longitudinal cross section with an upper side of 2 to 4cm, a lower side of 1 to 3cm, and a height of 1 to 3 cm.
6. The method of claim 1, wherein the substrate is selected from a metal substrate, a Si with SiO substrate 2 The substrate comprises a Si substrate, a sapphire substrate, a GaN substrate, an AlN substrate, an InN substrate, an AlGaN substrate and an InGaN substrate.
7. The method of claim 1, wherein in the step c), the catalyst is dissolved in a solvent to a solution with a concentration of 0.1 to 1mmol/L, and the solution is coated on the growth surface of the substrate and then dried by blowing or baking.
8. The preparation method of claim 1, wherein in step f), the temperature of the temperature zone A is raised to 150-300 ℃ at a heating rate of 10-30 ℃/min, the temperature of the temperature zone B is raised to 600-900 ℃ at a heating rate of 10-30 ℃/min, and the temperature is kept for 5-20 min.
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