CN117821938A - Growth equipment for realizing heterojunction of various two-dimensional materials and preparation method - Google Patents
Growth equipment for realizing heterojunction of various two-dimensional materials and preparation method Download PDFInfo
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- CN117821938A CN117821938A CN202410014165.8A CN202410014165A CN117821938A CN 117821938 A CN117821938 A CN 117821938A CN 202410014165 A CN202410014165 A CN 202410014165A CN 117821938 A CN117821938 A CN 117821938A
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- 239000000463 material Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title description 13
- 239000000758 substrate Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 27
- 230000005540 biological transmission Effects 0.000 claims description 17
- 230000007246 mechanism Effects 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010408 sweeping Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 32
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910021389 graphene Inorganic materials 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- 229910052582 BN Inorganic materials 0.000 description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 210000003437 trachea Anatomy 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BGECDVWSWDRFSP-UHFFFAOYSA-N borazine Chemical compound B1NBNBN1 BGECDVWSWDRFSP-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000009347 mechanical transmission Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal sulfides Chemical class 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
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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
-
- 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
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- 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)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides growth equipment for realizing heterojunctions of various two-dimensional materials, and particularly relates to the technical field of chemical vapor deposition, wherein the growth equipment for realizing heterojunctions of various two-dimensional materials comprises a sample table, a driving device, a fixing frame and a containing assembly, the containing assembly comprises a first inner tube, a second inner tube and a third inner tube, the containing assembly further comprises a containing tube, a containing cavity is arranged in the containing tube, and the first inner tube, the second inner tube and the third inner tube are positioned in the containing cavity; the sample platform is located the first inner tube inboard, and drive arrangement drives first inner tube, second inner tube and third inner tube respectively and removes to sample platform one side, and the substrate on the sample platform is accomplished two-dimensional material growth at first inner tube, second inner tube and third inner tube respectively afterwards, accomplishes different two-dimensional material growth respectively in through first inner tube, second inner tube and third inner tube, accomplishes multiple two-dimensional material growth in the same equipment simultaneously, can avoid causing the pollution to other growth pipe walls to lead to impurity adsorption again.
Description
Technical Field
The invention relates to the technical field of chemical vapor deposition, in particular to growth equipment for realizing heterojunction of various two-dimensional materials and a preparation method thereof.
Background
The single-layer graphene serving as a representative two-dimensional material has various excellent characteristics such as ultrahigh carrier mobility, high thermal conductivity, high mechanical strength, high light transmittance and the like, and has great application prospects in various fields such as optical devices, integrated circuits, aerospace and the like.
In recent decades, research on two-dimensional materials grows exponentially, besides graphene, a plurality of two-dimensional materials such as two-dimensional hexagonal boron nitride, transition group metal sulfide, black phosphorus and the like are sequentially prepared, the performance and application of the two-dimensional materials are greatly expanded, besides the research on the properties, growth, application and the like of a single two-dimensional material, a heterostructure formed by interaction of a plurality of two-dimensional materials is also a hotspot of the current research, for example, the graphene/h-BN vertical heterojunction plays a role in greatly increasing the carrier mobility of a device in the preparation of a field effect transistor, and the mobility of carriers in the graphene on silicon is far greater than that of the graphene.
The two-dimensional material synthesis method comprises a mechanical stripping method, a magnetron sputtering method, chemical vapor deposition and the like, wherein the mechanical stripping method is simple to operate and can easily obtain high-quality materials, but has the advantages of smaller size, poor control of the layer number, poor repeatability and lower yield, so that the practical application in mass production is greatly limited; the magnetron sputtering method has the advantages that the growth does not need a substrate catalysis effect, the preparation can be completed at normal temperature, the preparation speed is extremely high, but the problems of difficult target selection, high growth cost, poor material crystallization quality and the like exist, the mainstream two-dimensional material synthesis method in the market at present is a chemical vapor deposition method, the principle is that gaseous or steam substances are used as precursors and are conveyed to a rear-end high-temperature growth area, chemical reaction is carried out on the surface of the substrate to generate solid sediment, and the chemical vapor deposition method has the advantages of low cost, strong layer number controllability, suitability for large-area high-quality continuous film preparation and the like.
The main step of performing heterojunction chemical vapor deposition on a two-dimensional material by adopting a tubular furnace at present is to complete the growth of a first layer of two-dimensional material on a substrate in one growth device, then place a sample in a second special growth device for heterojunction synthesis, and in the process of transporting the sample from one device to the other device, impurities can be adsorbed to cause pollution, meanwhile, if multiple two-dimensional materials are continuously synthesized in a single device, different precursor sources generate chemical reactions at a rear-end high-temperature region, impurities can be adsorbed on the inner wall of the device, and serious interference and pollution can be caused to follow-up.
Disclosure of Invention
In order to solve the problem that impurities are easily adsorbed on a substrate or adsorbed on the inner wall of the device during heterojunction chemical vapor deposition preparation, the invention provides growth equipment for realizing a plurality of two-dimensional material heterojunction and a preparation method thereof.
The invention is realized by the following technical scheme:
the invention provides a growth device for realizing heterojunction of various two-dimensional materials, which comprises a sample table, a driving device, a fixing frame and a containing assembly, wherein:
the accommodating assembly comprises a first inner tube, a second inner tube and a third inner tube, wherein the first inner tube is positioned at the inner side of the second inner tube, the third inner tube is positioned at the outer side of the second inner tube, one sides of the first inner tube, the second inner tube and the third inner tube are respectively fixedly connected with the driving device, the accommodating assembly further comprises an accommodating tube, an accommodating cavity is formed in the accommodating tube, the first inner tube, the second inner tube and the third inner tube are positioned in the accommodating cavity, and the accommodating tube is fixed at one side of the top of the fixing frame;
the sample platform is located the first inner tube is inboard, the sample platform is used for holding the substrate, the sample platform supports fixedly through the arm, drive arrangement respectively drives first inner tube the second inner tube with the third inner tube moves to sample platform one side, later the substrate on the sample platform is in respectively first inner tube the second inner tube with the growth of two-dimensional material is accomplished to the third inner tube.
Further, still include vacuum apparatus, vacuum apparatus includes vacuum pump and outlet duct, the vacuum pump is located hold the subassembly and keep away from drive arrangement one side, the vacuum pump through the outlet duct with sample platform inner space communicates.
Further, a pressure gauge is arranged on the air outlet pipe and used for detecting the pressure value in the accommodating cavity.
Further, still include air supply device, air supply device includes mixing gas case and fortune trachea, fortune trachea one end with hold tub one side and be connected with hold the chamber and communicate with each other, the other end with mixing gas case is connected, mixing gas case is located the mount bottom is kept away from hold subassembly one side.
Further, an air inlet valve is further arranged on the air conveying pipe and used for controlling on-off of the air conveying pipe.
Further, a flowmeter is arranged on the gas conveying pipe and is used for detecting gas flow.
Further, the air control system is integrated with the air mixing box.
Further, the device also comprises a heating box, wherein the heating box is positioned at one side of the bottom of the accommodating pipe, and the heating box is fixedly connected with the fixing frame.
Further, the driving device comprises a gear transmission device, the transmission device comprises a plurality of telescopic rods and a transmission mechanism, the telescopic rods are arranged, one ends of the telescopic rods are respectively fixedly connected with the first inner tube, the second inner tube and the third inner tube, and the other ends of the telescopic rods are connected with the transmission mechanism.
Further, a preparation method of a growth device for realizing heterojunction of a plurality of two-dimensional materials comprises the following steps:
s1, placing a substrate in a sample stage, and sequentially carrying out vacuum and ventilation cavity scanning treatment on the inside of a containing tube;
s2, arranging a gas mixing box to respectively introduce different gas sources, and respectively arranging heating programs required by the growth of the different gas sources in a heating box;
s3, respectively completing growth of different two-dimensional materials in the first inner tube, the second inner tube and the third inner tube;
s4, stopping gas introduction, closing the gas mixing box and the heating box, and cooling to obtain a finished product.
The invention has the beneficial effects that:
the growth equipment for realizing the heterojunction of various two-dimensional materials provided by the invention is characterized in that the first inner tube, the second inner tube and the third inner tube are movably arranged, the accommodating tube is used for accommodating the first inner tube, the second inner tube and the third inner tube, the sample stage is arranged on the inner side of the third inner tube, and then the driving device is used for driving the three inner tubes to move, so that the sample stage can respectively complete the growth of different two-dimensional materials on different inner tubes, the growth of various two-dimensional materials can be completed in one equipment, and the phenomenon that impurities formed during the growth of different two-dimensional materials are adsorbed on the same inner wall to cause serious interference and pollution to subsequent reactions can be avoided.
Drawings
FIG. 1 is an overall block diagram of a growth apparatus implementing a plurality of two-dimensional material heterojunctions in accordance with the present invention;
FIG. 2 is a cross-sectional view of a containment assembly of a growth apparatus implementing a plurality of two-dimensional material heterojunctions in accordance with the present invention;
in the figure: the device comprises a containing assembly 1, a containing tube 11, a first inner tube 12, a second inner tube 13, a third inner tube 14, a driving device 2, a transmission mechanism 21, a telescopic rod 22, an air supply device 3, an air mixing box 31, an air conveying tube 32, a vacuum device 4, a vacuum pump 41, an air outlet tube 42, a heating box 5, a fixing frame 6 and a sample table 7;
the realization, functional characteristics and advantages of the present invention are further described with reference to the accompanying drawings in combination with the embodiments.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described below with reference to the accompanying drawings.
Referring to fig. 1-2, the present invention proposes a growth apparatus for realizing heterojunction of multiple two-dimensional materials, comprising a sample stage 7, a driving device 2, a fixing frame 6 and a receiving assembly 1, wherein:
the accommodating assembly 1 comprises a first inner tube 12, a second inner tube 13 and a third inner tube 14, wherein the first inner tube 12 is positioned at the inner side of the second inner tube 13, the third inner tube 14 is positioned at the outer side of the second inner tube 13, one sides of the first inner tube 12, the second inner tube 13 and the third inner tube 14 are respectively fixedly connected with the driving device 2, the accommodating assembly 1 further comprises an accommodating tube 11, an accommodating cavity is formed in the accommodating tube 11, the first inner tube 12, the second inner tube 13 and the third inner tube 14 are positioned in the accommodating cavity, and the accommodating tube 11 is fixed at one side of the top of the fixing frame 6;
the sample stage 7 is located inside the first inner tube 12, the sample stage 7 is used for accommodating a substrate, the sample stage 7 is supported and fixed through a mechanical arm, the driving device 2 drives the first inner tube 12, the second inner tube 13 and the third inner tube 14 to move to one side of the sample stage 7 respectively, and then the substrate on the sample stage 7 grows on the two-dimensional material in the first inner tube 12, the second inner tube 13 and the third inner tube 14 respectively.
In the present embodiment, the following is described.
The sample stage 7 is used for placing a substrate;
the driving device 2 is used for driving the first inner tube 12, the second inner tube 13 and the third inner tube 14 to move;
the accommodating tube 11 is used for providing an accommodating structure;
the first inner tube 12, the second inner tube 13 and the third inner tube 14 are respectively used for providing accommodating structures for different two-dimensional materials;
specifically, the holding tube 11 and the sample stage 7 are made of quartz, the supporting part for supporting the holding assembly 1 is arranged on the fixing frame 6, the supporting part supports the holding tube 11, sealing flanges are arranged at two sides of the holding tube 11, the right side of the holding tube 11 is a high-temperature area, the first inner tube 12, the second inner tube 13 and the third inner tube 14 are respectively connected with the driving device 2, the sample stage 7 is arranged in the third inner tube 14 through a mechanical supporting arm, the sample stage 7 is always kept from being influenced by the outside, a substrate is placed on the sample stage 7, the third inner tube 14, the second inner tube 13 and the first inner tube 12 are sequentially arranged outside the sample stage 7, when various two-dimensional materials are required to be continuously synthesized, the second inner tube 13 and the third inner tube 14 are firstly moved to one side of the holding cavity, then the substrate on the sample stage 7 firstly grows in a two-dimensional material in a closed space formed in the first inner tube 12, after the growth of a two-dimensional material is finished, the driving device 2 drives the first inner tube 12 to transversely move, and enables the first inner tube 12 to separate from the sample table 7, then the second inner tube 13 is moved until the sample table 7 is completely positioned inside the second inner tube 13, the substrate sample table 7 completes the growth of another two-dimensional material in a closed space formed inside the second inner tube 13, and in the same way, when the growth of a third two-dimensional material is required, the second inner tube 13 can be moved to one side, the third inner tube 14 is moved until the sample table 7 is positioned inside the third inner tube 14, the sample table 7 and the substrate form the closed space inside the third inner tube 14, the two-dimensional material growth can be completed by utilizing the single one of the first inner tube 12, the second inner tube 13 and the third inner tube 14 to the outside of the sample table 7, and continuous synthesis of a plurality of two-dimensional materials can be realized, and is not easy to pollute the subsequent reaction.
In one embodiment, more inner tubes such as fourth inner tube, fifth inner tube, sixth inner tube, etc. can be provided to complete continuous synthesis of more kinds of two-dimensional materials, the materials of the accommodating tube 11 and the sample stage 7 can be selected according to practical situations, and the substrate can be selected from copper foil, copper-nickel alloy, sapphire and Si/SiO 2 Etc.
Further, the vacuum device 4 is further included, the vacuum device 4 comprises a vacuum pump 41 and an air outlet pipe 42, the vacuum pump 41 is positioned on one side of the accommodating component 1 far away from the driving device 2, and the vacuum pump 41 is communicated with the inner space of the sample table 7 through the air outlet pipe 42;
the air outlet pipe 42 is provided with a pressure gauge which is used for detecting the pressure value in the accommodating cavity;
the air supply device 3 is further arranged, the air supply device 3 comprises an air mixing box 31 and an air conveying pipe 32, one end of the air conveying pipe 32 is connected with one side of the accommodating pipe 11 and communicated with the accommodating cavity, the other end of the air conveying pipe is connected with the air mixing box 31, and the air mixing box 31 is positioned at one side of the bottom of the fixing frame 6 far away from the accommodating assembly 1;
the system also comprises a pneumatic control system, wherein the pneumatic control system is integrated with the gas mixing box 31;
the gas pipe 32 is provided with a flowmeter for detecting the gas flow;
an air inlet valve is also arranged on the air conveying pipe 32 and is used for controlling the on-off of the air conveying pipe 32;
still include heating cabinet 5, heating cabinet 5 is located and holds pipe 11 bottom one side, heating cabinet 5 and mount 6 fixed connection.
In the present embodiment, the following is described.
The vacuum pump 41 is used for sucking air to provide a vacuum environment;
the gas mixing tank 31 is used for providing a plurality of gases;
the heating box 5 is used for heating the inside of the accommodating assembly 1;
specifically, the vacuum pump 41 communicates to the inside of the accommodating component 1 through the air outlet pipe 42, the vacuum pump 41 can pump out air, the airtight space where the sample table 7 is located is in a vacuum state, the air mixing box 31 is provided with an air control system, the air control system can set the supply rate of various different gases, the air conveying pipe 32 is provided with an air inlet valve, after the air inlet valve is opened, the space inside where the sample table 7 is located is in a sealed state due to the vacuum pump 41, therefore, the air can be conveyed to the inside of the accommodating component 1 through the air conveying pipe 32, and finally the heating box 5 heats the accommodating component 1 to raise the reaction temperature required by the growth of the two-dimensional material, and the growth of the two-dimensional material is completed.
In one embodiment, the actual number of the gas-carrying pipes 32 can be selected according to the actual situation, and can be one or a plurality of gas-carrying pipes, when the gas-carrying pipes are arranged in a plurality of gas-carrying pipes, the reaction gas and the inert gas for carrying can be separated, and the heat exhausting fan is arranged in the heating box 5, so that the rapid cooling after the growth of the two-dimensional material is finished can be facilitated, and the temperature overshoot phenomenon possibly occurring in the heating process can be reduced.
Further, the driving device 2 comprises a gear transmission device, the transmission device comprises a plurality of telescopic rods 22 and a transmission mechanism 21, the telescopic rods 22 are provided with a plurality of telescopic rods, one ends of the telescopic rods 22 are respectively fixedly connected with the first inner tube 12, the second inner tube 13 and the third inner tube 14, and the other ends of the telescopic rods are connected with the transmission mechanism 21.
In the present embodiment, the following is described.
The transmission mechanism 21 and the telescopic rod 22 are used for driving the accommodating assembly 1 to transversely move;
specifically, there are three telescopic rods 22, and three telescopic rods 22 are respectively and fixedly connected with the first inner tube 12, the second inner tube 13 and the third inner tube 14, and the telescopic rods 22 can stretch and retract, so that the telescopic rods 22 can drive the first inner tube 12, the second inner tube 13 or the third inner tube 14 connected with the telescopic rods 22 to transversely move when being shortened, and therefore the sample stage 7 is separated from the sample stage 7, and the sample stage 7 respectively grows two-dimensional materials in the first inner tube 12, the second inner tube 13 and the third inner tube 14 under the action of the driving device 2.
In one embodiment, the transmission mechanism 21 may adopt a gear type mechanical transmission structure or other structures, and the structure of the telescopic rod 22 may also be selected according to practical situations.
Further, the preparation method of the growth equipment for realizing the heterojunction of the plurality of two-dimensional materials comprises the following steps:
s1, placing a substrate in a sample table 7, and sequentially carrying out vacuumizing and ventilation cavity sweeping treatment on the inside of a containing tube 11;
s2, arranging a gas mixing box 31 to respectively introduce different gas sources, and respectively arranging heating programs required by the growth of the different gas sources in a heating box 5;
s3, finishing the growth of different two-dimensional materials in the first inner tube 12, the second inner tube 13 and the third inner tube 14 respectively;
s4, stopping gas introduction, closing the gas mixing box 31 and the heating box 5, and cooling to obtain a finished product.
Specifically, taking the preparation of an h-BN/Gra heterojunction on a metal substrate as an example, opening sealing flanges on the right sides of two sides of the accommodating tube 11, and placing a growth substrate on the sample table 7, wherein the substrate is copper foil with the thickness of 5cm x 5 cm;
closing the sealing flange on the right side, sending the sample stage 7 to the center of the accommodating tube 11 (at this time, since the first inner tube 12, the second inner tube 13 and the third inner tube 14 are on the same side, and the sample stage 7 is also on the center of the third inner tube 14) by the mechanical arm, and turning on the vacuum pump 41 to perform vacuum evacuation;
when the pressure in the accommodating cavity is reduced to a set value, the vacuum pump 41 is closed, the air inlet valves on the air mixing box 31 and the mixer pipe are opened, high-purity argon is introduced, and the air rate is set through the air control system on the air mixing box 31;
when the pressure in the accommodating cavity rises to normal pressure, closing the air inlet valves on the air mixing box 31 and the air conveying pipe 32, setting the speed of argon to 0 through the air control system on the air mixing box 31, and restarting the vacuum pump 41;
repeatedly vacuumizing to a certain pressure and introducing argon to normal pressure for more than three times, so that the cavity sweeping treatment of the high-flow high-purity argon in the equipment is realized;
heating the accommodating cavity by setting a heating program through the heating box 5, and raising the temperature to a reaction temperature required by the growth of the first two-dimensional material;
the corresponding telescopic rod 22 is pulled by the transmission mechanism 21, the second inner tube 13 and the third inner tube 14 are pulled to the front end of the main cavity, the supply rates of methane, high-purity argon and high-purity hydrogen are respectively set by the pneumatic control system on the gas mixing box 31, the gas inlet valves on the gas mixing box 31 and the gas carrying tube 32 are opened, gas is introduced, and graphene growth in the first inner tube 12 is started;
after the growth of the first layer of two-dimensional material graphene is finished, closing air inlet valves on the air mixing box 31 and the air conveying pipe 32, setting all gas rates to 0 through an air control system on the air mixing box 31, and adjusting a heating program in a heating box 5 body to enable the accommodating cavity to reach the temperature required by the growth of the second layer of two-dimensional material;
the corresponding telescopic rod 22 is adjusted through the transmission mechanism 21, the first inner tube 12 is pulled to one end of the accommodating cavity, and the second inner tube 13 is pushed into the outside of the sample table 7;
after the accommodating cavity reaches the temperature required by the hexagonal boron nitride of the second two-dimensional material, respectively setting the supply rates of borazine gas, high-purity argon gas and high-purity hydrogen gas through a control system on the gas mixing box 31, opening the gas inlet valves on the mixing box and the gas conveying pipe 32, and starting to grow hexagonal boron nitride;
after the growth is finished, closing air inlet valves on the air mixing box 31 and the air conveying pipe 32, setting all air rates to 0 through an air control system on the air mixing box 31, waiting for cooling of equipment, and taking out a sample after cooling.
In one embodiment, the invention may also be applicable to the preparation of graphene, hexagonal boron nitride, transition metal sulfides, and the like, two-dimensional materials that may be grown using gaseous precursors and vertical heterojunctions associated therewith.
Of course, the present invention can be implemented in various other embodiments, and based on this embodiment, those skilled in the art can obtain other embodiments without any inventive effort, which fall within the scope of the present invention.
Claims (10)
1. Growth equipment for realizing heterojunction of various two-dimensional materials, which is characterized by comprising a sample table, a driving device, a fixing frame and a containing assembly, wherein:
the accommodating assembly comprises a first inner tube, a second inner tube and a third inner tube, wherein the first inner tube is positioned at the inner side of the second inner tube, the third inner tube is positioned at the outer side of the second inner tube, one sides of the first inner tube, the second inner tube and the third inner tube are respectively fixedly connected with the driving device, the accommodating assembly further comprises an accommodating tube, an accommodating cavity is formed in the accommodating tube, the first inner tube, the second inner tube and the third inner tube are positioned in the accommodating cavity, and the accommodating tube is fixed at one side of the top of the fixing frame;
the sample platform is located the first inner tube is inboard, the sample platform is used for holding the substrate, the sample platform supports fixedly through the arm, drive arrangement respectively drives first inner tube the second inner tube with the third inner tube moves to sample platform one side, later the substrate on the sample platform is in respectively first inner tube the second inner tube with the growth of two-dimensional material is accomplished to the third inner tube.
2. The growth apparatus for achieving heterojunctions of multiple two-dimensional materials of claim 1, further comprising a vacuum device comprising a vacuum pump and an outlet tube, the vacuum pump being located on a side of the containment assembly remote from the drive device, the vacuum pump being in communication with the sample stage interior space through the outlet tube.
3. The growth apparatus for realizing heterojunction of multiple two-dimensional materials as claimed in claim 2, wherein a pressure gauge is arranged on the air outlet pipe, and the pressure gauge is used for detecting the pressure value inside the accommodating cavity.
4. The growth apparatus for achieving heterojunctions of multiple two-dimensional materials according to claim 1, further comprising an air supply device, wherein the air supply device comprises an air mixing box and an air transporting pipe, one end of the air transporting pipe is connected with one side of the accommodating pipe and communicated with the accommodating cavity, the other end of the air transporting pipe is connected with the air mixing box, and the air mixing box is located at one side, away from the accommodating assembly, of the bottom of the fixing frame.
5. The growth device for realizing heterojunction of multiple two-dimensional materials according to claim 4, wherein the gas carrying tube is further provided with a gas inlet valve, and the gas inlet valve is used for controlling on-off of the gas carrying tube.
6. The growth apparatus for implementing heterojunctions of multiple two-dimensional materials according to claim 5, wherein a flowmeter is provided on the gas carrying tube, the flowmeter being configured to detect the flow of gas.
7. The growth apparatus for achieving multiple two-dimensional material heterojunctions of claim 6, further comprising a pneumatic control system integrated with the gas mixing tank.
8. The growth apparatus for achieving heterojunctions of multiple two-dimensional materials of claim 1, further comprising a heating box, wherein the heating box is located at a bottom side of the receiving tube, and wherein the heating box is fixedly connected with the fixing frame.
9. The growth apparatus for implementing heterojunctions of multiple two-dimensional materials according to claim 1, wherein the driving device comprises a gear transmission device, the transmission device comprises a plurality of telescopic rods and a transmission mechanism, one ends of the telescopic rods are fixedly connected with the first inner tube, the second inner tube and the third inner tube respectively, and the other ends of the telescopic rods are connected with the transmission mechanism.
10. The method of manufacturing a growth device for achieving heterojunctions of a plurality of two-dimensional materials according to claims 1-9, comprising the steps of:
s1, placing a substrate in a sample table, and sequentially vacuumizing and ventilating and sweeping the inside of a containing tube;
s2, arranging a gas mixing box to respectively introduce different gas sources, and respectively arranging heating programs required by the growth of the different gas sources in a heating box;
s3, respectively completing growth of different two-dimensional materials in the first inner tube, the second inner tube and the third inner tube;
s4, stopping gas introduction, closing the gas mixing box and the heating box, and cooling to obtain a finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410014165.8A CN117821938A (en) | 2024-01-04 | 2024-01-04 | Growth equipment for realizing heterojunction of various two-dimensional materials and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410014165.8A CN117821938A (en) | 2024-01-04 | 2024-01-04 | Growth equipment for realizing heterojunction of various two-dimensional materials and preparation method |
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| Publication Number | Publication Date |
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| CN117821938A true CN117821938A (en) | 2024-04-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202410014165.8A Pending CN117821938A (en) | 2024-01-04 | 2024-01-04 | Growth equipment for realizing heterojunction of various two-dimensional materials and preparation method |
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| Country | Link |
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| CN (1) | CN117821938A (en) |
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- 2024-01-04 CN CN202410014165.8A patent/CN117821938A/en active Pending
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