CN111074234A - Device and method for growing two-dimensional material based on push-pull trolley mode - Google Patents

Device and method for growing two-dimensional material based on push-pull trolley mode Download PDF

Info

Publication number
CN111074234A
CN111074234A CN201911407064.2A CN201911407064A CN111074234A CN 111074234 A CN111074234 A CN 111074234A CN 201911407064 A CN201911407064 A CN 201911407064A CN 111074234 A CN111074234 A CN 111074234A
Authority
CN
China
Prior art keywords
reaction tube
gas
furnace
quartz boat
growing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201911407064.2A
Other languages
Chinese (zh)
Inventor
于佳鑫
曹元广
邢帅
吉妍
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Shanghai for Science and Technology
Original Assignee
University of Shanghai for Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Shanghai for Science and Technology filed Critical University of Shanghai for Science and Technology
Priority to CN201911407064.2A priority Critical patent/CN111074234A/en
Publication of CN111074234A publication Critical patent/CN111074234A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention provides a device for growing a two-dimensional material based on a push-pull trolley, which comprises: a reaction tube having an inlet end provided with an inlet flange and an outlet end provided with an outlet flange; a furnace disposed outside the reaction tube and adjacent to the outlet end side, having an upstream port and a downstream port; the trolley is provided with an arm rod and is placed in the reaction tube and close to one side of the inlet end; the magnet is arranged on the outer side of the reaction tube and is arranged above the trolley; the first quartz boat is placed in the reaction tube, is connected with the arm rod and is positioned at the upstream port of the furnace; a second quartz boat located at the center of the furnace; the substrate is buckled upside down above the second quartz boat; one end of the air inlet pipe is connected with the inlet flange, and the other end of the air inlet pipe is respectively connected with an Ar air inlet channel and H2An air intake passage; one end of the air outlet pipe is connected with the outlet flange, and the other end of the air outlet pipe is connected with an air pump. The invention also provides a method based on the push-pull trolleyA method for preparing a two-dimensional material for an apparatus for growing a two-dimensional material.

Description

Device and method for growing two-dimensional material based on push-pull trolley mode
Technical Field
The invention belongs to the technical field of growing two-dimensional materials, and particularly relates to a device and a method for growing two-dimensional materials based on a push-pull trolley mode.
Background
Two-dimensional (2D) materials are composed of a single or a small number of atomic or molecular layers, with stronger covalent or ionic bonds in the layers, and weaker van der waals bonds between the layers, with unique properties and functions due to their unique two-dimensional structure. In 2004, the Geim group obtained single-layer graphene by mechanical stripping, studied the relevant performance of the graphene, and triggered the research heat tide of two-dimensional materials, but the zero band gap property limited the application of graphene in the electronic field. And transition metal chalcogenides (TMDCs, including MoS)2、WSe2Etc.) extend the two-dimensional material beyond graphene, which brings hope for the application of the two-dimensional material. The single-layer TMDCs are used as a direct band gap semiconductor and have the characteristics of band gap adjustability, spin freedom degree, valley freedom degree controllability and the like, so that the single-layer TMDCs have wide application prospects in the fields of low-power-consumption electrons, flexible electrons, valley electronics, spin electrons and the like. Common methods for preparing TMDCs include ultrasonic liquid phase stripping, mechanical stripping, molecular beam epitaxy, chemical vapor deposition, and the like. The Chemical Vapor Deposition (CVD) method is one of the most important methods for preparing two-dimensional material films, can prepare large-size and high-quality single-layer TMDCs, and achieves the preparation purpose by regulating and controlling the amount and the proportion of precursors, the distance, the carrier gas flow, the growth temperature, the growth time and the like in the growth process. Albeit for a single layer of MoS2There are many more mature methods of preparation, the common method of growth being the substrate flipped over a boat containing the raw materials. But more excellent for all aspects of single layer WSe2The preparation method and growth mechanism of (2) are rarely studied. For growth of selenide materials, especially WSe2Preparation of precursor WO3High sublimation temperature, and intermediate product WxOyThe required temperature is generally in excess of 1060 ℃ and the intermediate product is reduced to WSe by Se2The reaction temperature is lower, about 500 ℃, and the temperature difference between the two steps is large, so that the WSe grows by the conventional back-off method at present2The main problems faced by materials are as follows: (1) if the furnace temperature is set to be higher, the precursor is sublimated at high temperature to generate an intermediate product, and the concentration of the raw material in the reaction tube is just suitable for WSe2Growing, but at the moment, the substrate temperature is far higher than the growth temperature, and the effective nucleation and crystallization cannot be realized; (2) if the furnace temperature is reduced to be proper for WSe2The precursor sublimation reaction rate does not provide the desired reactant concentration and growth is also inhibited.
Aiming at the great temperature difference of the two processes, one solution is to grow the WSe by placing the substrate at the downstream of a high-temperature furnace2. This approach can compromise solution to WSe2The growth temperature condition is problematic, but the concentration of the precursor is mainly concentrated near the raw material boat in the center of the furnace, and the concentration of the precursor reaching the downstream substrate is greatly reduced, so that the utilization rate of the raw material is sacrificed, and a good growth effect is difficult to achieve. In addition, there is another method that after the constant temperature operation of the high temperature furnace is finished, the high temperature furnace cover is opened to perform heat exchange between the furnace tube and the room temperature, so that the material is rapidly cooled to the growth temperature, but the cooling method cannot control the cooling range at one time and is not safe enough. In summary, in order to solve the contradiction between the sublimation temperature and the growth temperature of the precursor, rapid cooling is an indispensable step for growing a single-layer two-dimensional material with excellent growth quality, but no effective method for achieving rapid cooling exists at present.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide an apparatus and method for growing a two-dimensional material based on a push-pull cart.
The invention provides a device for growing two-dimensional materials based on a push-pull trolley, which is used for growing the two-dimensional materials and has the characteristics that: a reaction tube having an inlet end provided with an inlet flange and an outlet end provided with an outlet flange; the furnace is used for heating, is arranged on the outer side of the reaction tube, is close to one side of the outlet end, and is provided with an upstream port and a downstream port; the trolley is provided with an arm rod and is placed in the reaction tube and close to one side of the inlet end; the magnet is arranged on the outer side of the reaction tube, is arranged above the cart and is used for controlling the cart to move through magnetic force; a first quartz boat disposed in the reaction tube and connected to the arm, disposed at an upstream port of the furnace, for holding a quartz tubePlacing first precursor powder; the second quartz boat is positioned in the center of the furnace and used for placing second precursor powder; the substrate is reversely buckled above the second quartz boat and used for growing and obtaining a two-dimensional material; one end of the air inlet pipe is connected with the inlet flange, and the other end of the air inlet pipe is respectively connected with an Ar air inlet channel and H2The gas inlet channel is used for inputting corresponding gas; one end of the outlet pipe is connected with the outlet flange, the other end of the outlet pipe is connected with an air pump for pumping air, the inlet flange and the outlet flange are used for sealing the reaction pipe, the part of the furnace surrounding the reaction pipe is a reaction area, an Ar flow display instrument for adjusting the gas flow and an Ar gas cylinder for supplying gas are sequentially arranged in the Ar gas inlet channel, and H2H for adjusting gas flow is arranged in the gas inlet channel in sequence2Flow display instrument and H for air supply2The gas cylinder is also provided with an inlet valve for controlling the inflow of gas on the gas inlet pipe, and an outlet valve for controlling the outflow of gas on the gas outlet pipe.
The device for growing the two-dimensional material based on the push-pull trolley mode provided by the invention can also have the following characteristics: wherein the length of the reaction tube is 119.5 cm.
The device for growing the two-dimensional material based on the push-pull trolley mode provided by the invention can also have the following characteristics: wherein the length of the furnace is 53cm and the distance between the downstream port and the outlet end of the furnace is 20.5 cm.
The device for growing the two-dimensional material based on the push-pull trolley mode provided by the invention can also have the following characteristics: wherein, the length of the first quartz boat and the second quartz boat is 6 cm.
The device for growing the two-dimensional material based on the push-pull trolley mode provided by the invention can also have the following characteristics: wherein the first precursor powder is a chalcogenide element powder, and the second precursor powder is a transition metal oxide powder.
The device for growing the two-dimensional material based on the push-pull trolley mode provided by the invention can also have the following characteristics: wherein the height of the substrate from the second precursor powder is 1.5 cm.
The invention also provides a preparation method of the two-dimensional material, which adopts a device for growing the two-dimensional material based on the push-pull trolley, and is characterized by comprising the following steps: step 1, putting corresponding first precursor powder and second precursor powder into a first quartz boat and a second quartz boat according to a two-dimensional material to be prepared, placing the first quartz boat at an upstream port of a furnace, placing the second quartz boat at the central position of the furnace, and sealing a reaction tube through an inlet flange and an outlet flange;
step 2, after the reaction tube is sealed, opening an Ar flow display instrument, an inlet valve, an outlet valve and an air pump, pumping the interior of the reaction tube to a vacuum state, then opening an Ar gas cylinder, introducing high-purity Ar into the reaction tube, then closing the Ar gas cylinder, pumping the reaction tube to the vacuum state again, repeatedly introducing the high-purity Ar into the reaction tube, and pumping to the vacuum state twice to remove residual gas in the reaction tube;
step 3, after the residual gas is removed, opening an Ar gas cylinder, introducing high-purity Ar into the reaction tube, adjusting the flow of the Ar gas by an Ar flow indicator, and simultaneously adjusting an outlet valve to enable the pressure in the reaction tube to be close to the normal pressure of-0.0125 MPa;
step 4, opening the furnace to heat up, enabling the central temperature of the furnace to reach the sublimation temperature of the second precursor powder and enabling the upstream port to reach the sublimation temperature of the first precursor powder, and selecting whether to introduce H or not according to the preparation requirement of the two-dimensional material to be prepared2When H is required to be introduced2When it is turned on H2Gas cylinder and H2Flow indicator and adjust H2Flow rate display instrument, let H2Introducing into a reaction tube, and keeping introducing gas;
and 5, after the reaction area begins to be naturally cooled, controlling the cart to move through the magnet, rapidly pushing out the first quartz boat and the second quartz boat together, pushing the second quartz boat to the downstream port of the furnace, enabling the second quartz boat to be located at the growth temperature of the two-dimensional material to be prepared, and simultaneously closing the Ar flow display instrument, the Ar gas cylinder and the H gas cylinder2Flow indicator, H2Gas cylinder, inlet valve, outlet valve, air pump and stoveAnd naturally cooling the reaction area to room temperature in a sealed environment, and then preparing the required two-dimensional material on the substrate.
Action and Effect of the invention
According to the device and the method for growing the two-dimensional material based on the push-pull trolley, the magnet is arranged to push the trolley, so that when the second quartz boat sublimates in the center of the furnace to generate an intermediate product, the second quartz boat and the substrate are quickly pushed to the downstream port of the furnace together to meet the requirement of the growth temperature of the two-dimensional material, the second quartz boat is pushed to change the position to quickly cool, the contradiction that the temperature difference between the sublimation temperature of the precursor and the growth temperature of the two-dimensional material is large is solved, and meanwhile, the concentration of the reactant is kept at a high level due to the fact that the intermediate product is concentrated in the second quartz boat, and the success rate of preparing the two-dimensional material is improved. Therefore, the device and the method for growing the two-dimensional material based on the push-pull trolley can safely and effectively control the cooling amplitude, can ensure the concentration of reactants, improve the utilization rate of raw materials, improve the success rate of the preparation of the two-dimensional material, realize the preparation of a single-layer two-dimensional material, and can obtain the two-dimensional material with excellent surface quality.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for growing two-dimensional materials in a push-pull cart-based manner in an embodiment of the present invention;
FIG. 2 is a schematic structural view of a first quartz boat in an embodiment of the present invention;
FIG. 3 is a schematic structural view of a second quartz boat in an embodiment of the present invention;
FIG. 4 is a single layer WSe prepared in an example of the present invention2An optical microscope image of (a);
FIG. 5 is a single layer WSe prepared in an example of the present invention2PL spectra under 532nm excitation light source.
Detailed Description
In order to make the technical means and functions of the present invention easy to understand, the present invention is specifically described below with reference to the embodiments and the accompanying drawings.
Fig. 1 is a schematic structural diagram of an apparatus for growing two-dimensional materials based on a push-pull trolley manner in an embodiment of the present invention.
As shown in fig. 1, an apparatus 100 for growing two-dimensional material based on a push-pull cart in this embodiment is used for growing two-dimensional material, and includes: the device comprises a reaction tube 1, a furnace 2, a cart 3, a magnet 4, a first quartz boat 5, a second quartz boat 6, a substrate 7, an air inlet pipe 8 and an air outlet pipe 9.
The reaction tube 1 has an inlet end provided with an inlet flange 11 and an outlet end provided with an outlet flange 12.
The inlet flange 11 and the outlet flange 12 are used to seal the reaction tube 1.
In this example, the length of the reaction tube was 119.5 cm.
The furnace 2 is used for raising the temperature, is arranged outside the reaction tube 1 and near the outlet end side, and has an upstream port and a downstream port.
The portion of the furnace 2 surrounding the reaction tube 1 is a reaction zone.
In this example, the length of the furnace 2 was 53cm, and the distance between the downstream port and the outlet end of the furnace 2 was 20.5 cm.
The cart 3 is provided with an arm 31 placed inside the reaction tube 1 near the inlet end side.
The magnet 4 is arranged outside the reaction tube 1 and above the cart 3, and is used for controlling the cart 3 to move through magnetic force.
A first quartz boat 5 is placed in the reaction tube 1 and connected to the arm 31 at the upstream port of the furnace 2 for placing the first precursor powder.
FIG. 2 is a schematic structural diagram of a first quartz boat in an embodiment of the invention.
As shown in fig. 2, the first quartz boat 5 is uniformly and flatly laid with the first precursor powder 51 at the center.
A second quartz boat 6 is located at the center of the furnace 2 for placing the second precursor powder 61.
In this embodiment, the lengths of the first quartz boat 5 and the second quartz boat 6 are both 6 cm.
The first precursor powder 51 is a chalcogen powder, the second precursor powder 61 is a transition metal oxide powder, and the first precursor powder 51 and the second precursor powder 61 react to produce a transition metal chalcogenide.
FIG. 3 is a schematic structural diagram of a second quartz boat in an embodiment of the invention.
As shown in FIG. 3, in the present embodiment, the substrate 7 is coated with 300nm SiO three pieces2The Si composition of the layer, the substrate 7 is turned over the second quartz boat 6 for growth and obtaining of two-dimensional material, and the second quartz boat 6 is evenly and flatly paved with the second precursor powder 61.
The height of the substrate 7 from the second precursor powder was 1.5 cm.
Substrate 7 includes, but is not limited to, 300nm SiO plated2A Si substrate and a sapphire substrate of the layer.
One end of the air inlet pipe 8 is connected with the inlet flange 11, and the other end is respectively connected with an Ar air inlet channel 81 and an H2And an intake passage 82 for inputting the corresponding gas.
The inlet pipe 8 is also provided with an inlet valve 83 for controlling the inflow of gas.
An Ar flow rate display 811 for adjusting the flow rate of the gas and an Ar gas cylinder 812 for supplying the gas are sequentially provided in the Ar gas inlet passage 81,
H2h for regulating the gas flow is arranged in the gas inlet channel 82 in sequence2Flow indicator 821 and H for air supply2 A gas cylinder 822.
One end of the air outlet pipe 9 is connected with the outlet flange 12, and the other end is connected with an air extracting pump 91 for extracting air.
The outlet pipe 9 is also provided with an outlet valve 92 for controlling the outflow of the gas.
In the two-dimensional material preparation method using the push-pull cart based device 100 for growing a two-dimensional material in this embodiment, Se powder is selected as the first precursor powder 51, and WO3The powder is used as a second precursor powder 61 to prepare a two-dimensional material WSe2The method comprises the following steps:
step 1, uniformly spreading 120mgSe powder (99.9%) on the center of a first quartz boat 5, and then carrying out surface treatment on the quartz boat1mgWO3The powder (99.9%) was evenly spread in the center of the second quartz boat 6, and the substrate 7 was turned upside down over the second quartz boat 6, the first quartz boat 5 was placed at the upstream port of the furnace 2, the second quartz boat 6 was placed at the center of the furnace 2, and the reaction tube 1 was sealed by the inlet flange 11 and the outlet flange 12.
And 2, after the reaction tube 1 is sealed, opening an Ar flow display instrument 811, an inlet valve 83, an outlet valve 92 and an air pump 91, pumping the interior of the reaction tube 1 to a vacuum state, then opening an Ar gas cylinder 812, introducing high-purity Ar with the flow of 200sccm into the reaction tube for 15min, then closing the Ar gas cylinder 812, pumping the reaction tube 1 to the vacuum state again, and repeatedly introducing the high-purity Ar into the reaction tube 1 and pumping to the vacuum state twice to remove residual gas in the reaction tube 1.
Step 3, after the residual gas is removed, opening an Ar gas cylinder 812, introducing high-purity Ar into the reaction tube 1, adjusting the flow of the Ar gas to 80sccm through an Ar flow display 811, and simultaneously adjusting an outlet valve 92 to enable the pressure in the reaction tube 1 to be close to the normal pressure of-0.0125 MPa;
step 4, opening the furnace 2, raising the temperature at the speed of 25 ℃/min, and when the central temperature of the furnace reaches 900 ℃, keeping 1mgWO in the second quartz boat 63The powder (99.9%) undergoes sublimation to form the reactant, at which point H is reopened2 Gas cylinder 822 and H2Flow indicator 821 and adjust H2Flow rate display instrument, let H2Introducing into the reaction tube 1 at a flow rate of 5sccm, wherein Ar/H in the reaction tube 12The flow rate ratio of (1) was 80sccm/5sccm, and the flow was kept for 6 min.
In this example, when the temperature of the center of the furnace 2 reached 900 ℃, the temperature at the upstream port of the furnace 2 was 270 ℃ and 120mgSe powder (99.9%) in the first quartz boat 5 was melted.
Step 5, after the reaction zone begins to naturally cool down, when the temperature is reduced to 800 ℃, the magnet 4 controls the cart 3 to move, the first quartz boat 5 and the second quartz boat 6 are rapidly pushed out together, the second quartz boat 6 is pushed to the downstream port of the furnace 2, and the second quartz boat 2 is positioned at the WSe2At the growth temperature, the Ar flow display instrument 8 is closed11. Ar gas cylinder 812, H2Flow indicator 821, H2Gas cylinder 822, inlet valve 83, outlet valve 92, air pump 91 and furnace 2, so that the reaction area is naturally cooled to room temperature in a sealed environment, and WSe is prepared on substrate 72。
FIG. 4 is a single layer WSe prepared in an example of the present invention2FIG. 5 is an optical microscope image of a single layer WSe prepared in an example of the present invention2PL spectra under 532nm excitation light source.
In FIG. 4, a, b, and c are optical microscope images at different magnifications, respectively, and the magnifications are sequentially increased.
As shown in FIGS. 4 and 5, this example successfully produced a large-area triangular single-layer WSe with large transverse dimension, small and uniform thickness, less defects, and high quality2Crystals, WSe prepared2The transverse length of the crystal can reach 40-50 μm, and the thickness range is 0.7-0.9 nm.
Effects and effects of the embodiments
According to the device and the method for growing the two-dimensional material in the push-pull trolley based mode, the magnet is arranged to push the trolley, so that when the second quartz boat sublimates in the center of the furnace to generate an intermediate product, the second quartz boat and the substrate are quickly pushed to the downstream port of the furnace together to meet the requirement of the growth temperature of the two-dimensional material, the second quartz boat is pushed to change positions to quickly cool, the contradiction that the temperature difference between the sublimation temperature of the precursor and the growth temperature of the two-dimensional material is large is solved, meanwhile, the concentration of the reactant is guaranteed to be kept at a high level due to the fact that the intermediate product is concentrated in the second quartz boat, and therefore the success rate of preparing the two-dimensional material is improved. Therefore, the device and the method for growing the two-dimensional material based on the push-pull trolley can safely and effectively control the cooling range, can ensure the concentration of reactants, improve the utilization rate of raw materials, improve the success rate of two-dimensional material preparation, realize preparation of a single-layer two-dimensional material, and can obtain the two-dimensional material with excellent surface quality.
Furthermore, different two-dimensional materials can be correspondingly prepared by placing different precursor powders in the first quartz boat and the second quartz boat, so the method has wide application range and can be applied to the preparation of various two-dimensional materials.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.

Claims (7)

1. A device for growing two-dimensional materials based on a push-pull trolley mode is used for growing the two-dimensional materials and is characterized by comprising:
a reaction tube having an inlet end provided with an inlet flange and an outlet end provided with an outlet flange;
the furnace is used for heating, is arranged on the outer side of the reaction tube, is close to one side of the outlet end, and is provided with an upstream port and a downstream port;
the trolley is provided with an arm rod and is placed in the reaction tube and close to one side of the inlet end;
the magnet is arranged on the outer side of the reaction tube, is arranged above the cart and is used for controlling the cart to move through magnetic force;
the first quartz boat is placed in the reaction tube, connected with the arm rod, positioned at the upstream port of the furnace and used for placing first precursor powder;
the second quartz boat is positioned in the center of the furnace and used for placing second precursor powder;
the substrate is reversely buckled above the second quartz boat and used for growing and obtaining the two-dimensional material;
one end of the air inlet pipe is connected with the inlet flange, and the other end of the air inlet pipe is respectively connected with an Ar air inlet channel and H2The gas inlet channel is used for inputting corresponding gas;
one end of the air outlet pipe is connected with the outlet flange, the other end of the air outlet pipe is connected with an air pump for pumping air,
wherein the inlet flange and the outlet flange are used for sealing the reaction tube,
the part of the furnace surrounding the reaction tube is a reaction area,
an Ar flow display instrument for adjusting the gas flow and an Ar gas cylinder for supplying gas are sequentially arranged in the Ar gas inlet channel,
said H2H for adjusting gas flow is arranged in the gas inlet channel in sequence2Flow display instrument and H for air supply2A gas cylinder is arranged on the top of the gas cylinder,
the gas inlet pipe is also provided with an inlet valve for controlling the gas to flow in,
and the outlet pipe is also provided with an outlet valve for controlling the gas to flow out.
2. The cart-based apparatus for growing two-dimensional materials of claim 1, wherein:
wherein the length of the reaction tube is 119.5 cm.
3. The cart-based apparatus for growing two-dimensional materials of claim 1, wherein:
wherein the length of the furnace is 53cm,
the downstream port of the furnace is at a distance of 20.5cm from the outlet end.
4. The cart-based apparatus for growing two-dimensional materials of claim 1, wherein:
wherein the lengths of the first quartz boat and the second quartz boat are both 6 cm.
5. The cart-based apparatus for growing two-dimensional materials of claim 1, wherein:
wherein the first precursor powder is a chalcogenide powder,
the second precursor powder is transition metal oxide powder.
6. The cart-based apparatus for growing two-dimensional materials of claim 1, wherein:
wherein the substrate is 1.5cm in height from the second precursor powder.
7. A method for preparing a two-dimensional material using the cart-based device for growing a two-dimensional material according to claim 1, comprising the steps of:
step 1, putting corresponding first precursor powder and second precursor powder into a first quartz boat and a second quartz boat according to the two-dimensional material to be prepared, putting the first quartz boat at the upstream port of the furnace, putting the second quartz boat at the central position of the furnace, and sealing the reaction tube through the inlet flange and the outlet flange;
step 2, after the reaction tube is sealed, opening the Ar flow display instrument, the inlet valve, the outlet valve and the air pump, pumping the interior of the reaction tube to a vacuum state, then opening the Ar gas cylinder, introducing high-purity Ar into the reaction tube, then closing the Ar gas cylinder, pumping the reaction tube to the vacuum state again, and repeatedly introducing high-purity Ar into the reaction tube and pumping to the vacuum state twice to remove residual gas in the reaction tube;
step 3, after the residual gas is removed, opening the Ar gas cylinder, introducing high-purity Ar into the reaction tube, adjusting the flow of the Ar gas by the Ar flow indicator, and adjusting the outlet valve to enable the gas pressure in the reaction tube to be close to the normal pressure of-0.0125 MPa;
step 4, opening the furnace to heat up, enabling the central temperature of the furnace to reach the sublimation temperature of the second precursor powder and enabling the upstream port to reach the sublimation temperature of the first precursor powder, and selecting whether to introduce H or not according to the preparation requirement of the two-dimensional material to be prepared2When H is required to be introduced2When is turned on, the H2Gas cylinder and said H2Flow indicator and adjust H2Flow rate display instrument, let H2Introducing into the reaction tube, and keeping introducing gas;
and 5, after the reaction zone begins to naturally cool down, controlling the cart to move through the magnet, rapidly pushing out the first quartz boat and the second quartz boat together, pushing the second quartz boat to the downstream port of the furnace, enabling the second quartz boat to be located at the growth temperature of the two-dimensional material to be prepared, and simultaneously closing the Ar flow display instrument, the Ar gas cylinder and the H gas cylinder2Flow display instrument, said H2The gas cylinder, the inlet valve, the outlet valve, the air pump and the furnace enable the reaction area to be naturally cooled to room temperature in a sealed environment, and then the required two-dimensional material is prepared on the substrate.
CN201911407064.2A 2019-12-31 2019-12-31 Device and method for growing two-dimensional material based on push-pull trolley mode Pending CN111074234A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911407064.2A CN111074234A (en) 2019-12-31 2019-12-31 Device and method for growing two-dimensional material based on push-pull trolley mode

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911407064.2A CN111074234A (en) 2019-12-31 2019-12-31 Device and method for growing two-dimensional material based on push-pull trolley mode

Publications (1)

Publication Number Publication Date
CN111074234A true CN111074234A (en) 2020-04-28

Family

ID=70320420

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911407064.2A Pending CN111074234A (en) 2019-12-31 2019-12-31 Device and method for growing two-dimensional material based on push-pull trolley mode

Country Status (1)

Country Link
CN (1) CN111074234A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113355657A (en) * 2021-05-27 2021-09-07 天津大学 Source-dividing positioning vacuum tube furnace device

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105272358A (en) * 2015-06-01 2016-01-27 湘潭大学 Preparation method for a large-area single-layer or few-layer molybdenum disulfide film
CN106757361A (en) * 2016-11-14 2017-05-31 西安电子科技大学 MoS is grown based on CVD2The method of two dimensional crystal
CN107093560A (en) * 2017-04-19 2017-08-25 湖南大学 A kind of bismuth iodide two-dimensional material, preparation and its application
CN108193277A (en) * 2018-01-26 2018-06-22 西安电子科技大学 The method for preparing two tungsten selenide monocrystalline of large area individual layer

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105272358A (en) * 2015-06-01 2016-01-27 湘潭大学 Preparation method for a large-area single-layer or few-layer molybdenum disulfide film
CN106757361A (en) * 2016-11-14 2017-05-31 西安电子科技大学 MoS is grown based on CVD2The method of two dimensional crystal
CN107093560A (en) * 2017-04-19 2017-08-25 湖南大学 A kind of bismuth iodide two-dimensional material, preparation and its application
CN108193277A (en) * 2018-01-26 2018-06-22 西安电子科技大学 The method for preparing two tungsten selenide monocrystalline of large area individual layer

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113355657A (en) * 2021-05-27 2021-09-07 天津大学 Source-dividing positioning vacuum tube furnace device
CN113355657B (en) * 2021-05-27 2022-10-28 天津大学 Source-dividing positioning vacuum tube furnace device

Similar Documents

Publication Publication Date Title
CN103194729B (en) The preparation method of metal chalcogenide film
CN109371381B (en) Method for preparing single-layer molybdenum sulfide/tungsten sulfide in-plane heterojunction by low-temperature one-step method
CN107299333A (en) A kind of preparation method of single-layer molybdenum disulfide film
CN113428845B (en) Method for preparing two-dimensional molybdenum ditelluride nano material by limited-area chemical vapor deposition
CN110551986B (en) Method for direct patterned growth of atomic layer transition metal dichalcogenides
CN112359421B (en) Method for preparing layered bismuth-oxygen-selenium semiconductor film by reverse airflow method
WO2021129450A1 (en) Method for preparing uniform material layer based on chemical vapor deposition
CN112921297B (en) CVD preparation method of ferromagnetic two-dimensional material FeGeTe
CN112501555A (en) Preparation method of single-layer molybdenum disulfide film
CN112695381A (en) Method for rapidly growing ultrathin large-size single crystal transition metal sulfur/selenide
CN113122818B (en) Method for preparing wafer-level single-layer molybdenum disulfide film
CN111074234A (en) Device and method for growing two-dimensional material based on push-pull trolley mode
CN112456452B (en) Preparation method of germanium diselenide nano material
CN110804731B (en) Mn grown by atomic layer deposition technologyxN film method
CN110835747A (en) Method for regulating and controlling morphology and defects of molybdenum disulfide through temperature
Wong Chemical vapor deposition growth of 2D semiconductors
CN111519186B (en) Ferromagnetic/graphene epitaxial interface and low-temperature preparation method thereof
Yanase et al. Chemical vapor deposition of MoS2: Insight into the growth mechanism by separated gas flow experiments
TWI518198B (en) System for preparing films
CN113584458A (en) Method for preparing diamond film on potassium tantalate niobate crystal by microwave plasma chemical vapor deposition technology
CN109898070A (en) A kind of preparation method of tungsten disulfide molecule layer film
CN201826011U (en) Water vapor expanding device for growth of oxide semiconductor thin film
CN115341272B (en) Preparation method of millimeter-level two-dimensional topological material bismuth selenide monocrystal
CN111285402A (en) Preparation method of single-layer transition metal sulfide
CN113981542B (en) Method for preparing high-quality single-crystal-domain two-dimensional material by regulating and controlling cavity pressure

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200428