CN115807215A - MOCVD device and method for preparing two-dimensional crystal material based on ultrasonic atomization - Google Patents
MOCVD device and method for preparing two-dimensional crystal material based on ultrasonic atomization Download PDFInfo
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Abstract
The invention discloses an MOCVD device and a method for preparing a two-dimensional crystal material based on ultrasonic atomization, belonging to the field of preparation of two-dimensional crystal materials, wherein the MOCVD device comprises: a sample stage and an ultrasonic atomization nozzle are arranged in the reaction chamber; the first atomization device is used for placing a liquid first raw material and directly atomizing the first raw material to generate vapor of the first raw material; the second atomization device is used for placing a solid second raw material and heating the second raw material to generate steam of the second raw material; the technical scheme of the invention can effectively solve the problems that the source is liquefied into large-particle liquid drops in the transportation process and the static gas mixing effect is poor in the preparation process of the two-dimensional crystal material, so that the preparation precision of the material is high, the uniformity and the repeatability of the product are good, and the application range of the chemical vapor deposition equipment is wide.
Description
Technical Field
The invention belongs to the field of preparation of two-dimensional crystal materials, and particularly relates to an MOCVD device and method for preparing a two-dimensional crystal material based on ultrasonic atomization.
Background
MOCVD (Metal-Organic Chemical Vapor Deposition) is a Chemical Vapor phase epitaxy (cvd) technique developed on the basis of Vapor Phase Epitaxy (VPE) technique. The method is provided by Manasevit of Rockwell corporation in 1968, rapidly develops from the 80 th of 20 th century, and shows great superiority in preparing two-dimensional semiconductor heterojunction materials, organic compounds of III group and II group elements and hydrides of V group and VI group elements are taken as source materials, are carried by carrier gas and conveyed into a reaction chamber, generate corresponding chemical reaction on the surface of a heated substrate, generate various III-V group and II-VI group compound two-dimensional atomic crystal materials, and deposit on the substrate, thereby obtaining corresponding epitaxial two-dimensional crystal film materials.
At present, MOCVD (metal organic chemical vapor deposition) is mainly used for conveying solid or liquid sources, the solid or liquid sources are heated and evaporated through a water bath and then are conveyed to a reaction chamber by using a carrier gas, the process limits the types of non-gaseous sources, and the source is easily condensed into small liquid drops or the source adsorption tube wall in the conveying process, so that the utilization rate of source materials is low. In addition, the gas mixer who uses in two-dimensional crystal material growth field is static mixer mostly, and its theory of operation is that several ways of gas are through airtight space simple collision then realize mixing, and the mixing effect depends on the structure in gas mixing chamber space, the relatively poor problem of ubiquitous gas mixing effect. Therefore, it is necessary to design advanced organic source transport devices and dynamic gas mixing devices to meet MOCVD, which is required for integrated large-area production of two-dimensional atomic crystal semiconductor processes.
Disclosure of Invention
The invention provides an MOCVD device and a method for preparing a two-dimensional crystal material based on ultrasonic atomization, which are provided with an advanced organic source conveying device and a dynamic gas mixing device and solve the problems of poor gas mixing effect and low source material utilization rate in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
an MOCVD device for preparing a two-dimensional crystal material based on ultrasonic atomization comprises: the device comprises a gas source channel, a non-gaseous source atomization channel, an ultrasonic atomization nozzle and a reaction chamber; outlets of the gas source channel and the non-gaseous source atomization channel are respectively connected with an inlet of an ultrasonic atomization nozzle, the outlet of the ultrasonic atomization nozzle is positioned at the top end of the inner part of the reaction chamber, and a sample stage is arranged at the position, right below the ultrasonic atomization nozzle, of the bottom end of the inner part of the reaction chamber;
the non-gaseous source atomizing channel is composed of a plurality of liquid source atomizing channels, solid source atomizing channels or two channels;
a liquid source atomizing device is arranged in the liquid source atomizing channel and comprises a container, an ultrasonic micropore atomizing sheet, liquid absorbing cotton and a cover; the cover is in a step shape, the bottom end of the cover is clamped at the outer side of the top end of the container, an ultrasonic micropore atomization sheet is arranged above the contact part of the cover and the container, damping rubber is arranged between the ultrasonic micropore atomization sheet and the cover, and a carrier gas inlet is arranged on the side surface of the cover above the ultrasonic micropore atomization sheet; an outlet is arranged at the top of the cover; the liquid absorption cotton is positioned in the container, the bottom of the liquid absorption cotton is arranged in the liquid source, and the top of the liquid absorption cotton is connected with the metal sheet of the through hole array on the ultrasonic micropore atomization sheet; the liquid source is transmitted to the metal sheet of the through hole array in the ultrasonic micropore atomization sheet through the liquid absorption cotton, and the metal sheet is driven by the piezoelectric ceramics to vibrate at high frequency to atomize to smaller particles and even vaporize;
a solid source atomization device is arranged in the solid source atomization channel and comprises a container, a high-temperature-resistant driver and a cover; the cover is in a step shape, the bottom end of the cover is clamped at the outer side of the top end of the container, a high-temperature-resistant ultrasonic micropore atomization sheet is arranged above the contact part of the cover and the container, a high-temperature-resistant damping block is arranged between the high-temperature-resistant ultrasonic micropore atomization sheet and the cover, and a carrier gas inlet is arranged on the side surface of the cover above the high-temperature-resistant ultrasonic micropore atomization sheet; an outlet is arranged at the top of the cover; the bottom of the container is provided with a heating base, the solid source is placed on the heating base, the solid source is evaporated to a metal sheet of a through hole array in the high-temperature-resistant ultrasonic microporous atomization sheet through heating, and the metal sheet is driven by piezoelectric ceramics to vibrate at high frequency to further atomize to smaller particles and even vaporize;
the ultrasonic atomizing nozzle comprises a gas mixing chamber, a high-temperature-resistant ultrasonic micropore atomizing sheet and a frustum-shaped shield; the top end of the gas mixing chamber is provided with a plurality of gas inlets for connecting the outlets of the gaseous source channel and the non-gaseous source atomization channel, the bottom end of the gas mixing chamber is convexly provided with high-temperature resistant ultrasonic micropore atomization sheets towards two sides, a high-temperature resistant damping block is arranged between the high-temperature resistant ultrasonic micropore atomization sheets and the inner wall of the gas mixing chamber, and the bottom end of the gas mixing chamber is positioned below the high-temperature resistant ultrasonic micropore atomization sheets and is provided with a frustum-shaped shield;
the ultrasonic micropore atomization sheet consists of high-temperature-resistant annular piezoelectric ceramic and a metal sheet with a conical hole, wherein one end of a large hole of the conical hole is a liquid inlet, the other end of a small hole of the conical hole is a gas outlet, the annular piezoelectric ceramic is attached to one surface of a large hole of the metal sheet, the aperture of the large hole is 5-20 mu m, and the aperture of the small hole is 1-5 mu m;
the vertical distance between the small hole of the ultrasonic micropore atomization sheet in the ultrasonic atomization nozzle and the sample platform is 5-100 mm, when liquid drops flow from the large hole to the small hole, the flow rate of the liquid drops is increased, the liquid drops flow from the small hole to the large hole, the flow rate of the liquid drops is decreased, the liquid drops are slowly gathered in the large hole, and after ultrasonic vibration is added, cavitation or micro shock waves are generated to atomize the liquid; when the liquid source reaches the large holes on the metal sheet through the liquid absorption cotton or the solid source reaches the large holes on the metal sheet through evaporation, the piezoelectric ceramic drives the metal sheet to vibrate up and down at the frequency of MHz level, liquid drops and the metal sheet generate rapid relative motion, the liquid source or the solid source of large-particle smog enters the large holes and is rapidly converted into fine-particle smog to be sprayed out, the fine liquid drops are carried to the substrate of the reaction chamber through carrier gas, the thicker liquid drops are generally continuously gasified by a cavitation field generated on the upper surface of the vibrated metal sheet or flow back to accumulate the large holes on the back of the metal sheet, and the liquid drops with certain size are continuously sprayed out from the small holes through ultrasonic cavitation; the sample stage can rotate and be adjusted up and down, and the rotating speed is 100-300 r/min.
The method for preparing the two-dimensional crystal material by adopting the device comprises the following steps:
firstly, reaction gas from a solid or liquid source is subjected to preliminary ultrasonic refinement, then is conveyed to the upper part of an ultrasonic atomizing nozzle through a carrier gas in a gas inlet pipeline, and is quickly sprayed onto the surface of a substrate of an MOCVD reaction chamber through a cone through hole array of an atomizer. After entering the MOCVD reaction chamber, the substrate rotates along with the substrate tray, so that different reaction gases can be contacted above the substrate in a short time accumulation range in a cycle, the surface of the epitaxial layer is kept in a uniform mixing state, the migration of a source on the surface of the epitaxial layer is greatly improved, and the method is particularly favorable for growing single-component or multi-component two-dimensional crystal materials.
The two-dimensional crystal material includes: single element two-dimensional crystal material boron alkene, graphene, transition metal sulfur group two-dimensional crystal material MX 2 And III-VI two-dimensional crystal material VX, wherein M is a transition metal element, X is a chalcogen element, and V is a third main group element.
The solid raw material comprises: one or a mixture of more than two of sodium borohydride, lithium borohydride, potassium borohydride, sodium boron deuteride, sodium cyanoborohydride, tetramethylammonium borohydride, tetramethylammonium triacetoxyborohydride, lithium tri-sec-butylborohydride, cuprous bis (triphenylphosphine) borohydride, tetrabutylammonium borohydride, lithium triethylborohydride, lithium tri-sec-butylborohydride, lithium tripentyl borohydride, potassium tri (3, 5-dimethyl-1-pyrazolyl) borohydride, tetra-n-butylammonium borohydride, potassium triisobutylborohydride and benzyltriphenylphosphine borohydride;
the first raw material comprises: dimethyldisulfide, diethylsulfide, diethyldiselenide, hydrogen sulfide, hydrogen selenide, sulfur, selenium, the second raw material comprising: molybdenum dimethyldithiocarbamate, bis (tert-butylamine) bis (dimethylamine) tungsten, hexahydroxymolybdenum, hexahydroxytungsten, tungsten hexachloride, trimethylindium, indium trichloride;
the substrate is metal such as gold, silver, copper, aluminum, iridium, rubidium and the like, or nonmetal such as mica, quartz plate, silicon chip, glass, silicon carbide, silicon boride, sapphire, gallium nitride, gallium arsenide, gallium oxide, graphene, boron nitride, molybdenum sulfide, tungsten sulfide, molybdenum selenide, tungsten selenide, antimony selenide, bismuth sulfide, bismuth telluride, antimony telluride, magnesium oxide, magnesium boride, titanium boride, calcium boride, aluminum boride and the like.
The carrier gas is hydrogen, hydrogen-argon, hydrogen-nitrogen mixed gas, high-purity nitrogen, argon or hydride gas, and the flow rate of the carrier gas is less than or equal to 100sccm.
The growth temperature of the two-dimensional crystal material is 500-1000 ℃, and the thickness of the two-dimensional crystal material is accurately controlled from a monoatomic layer to 20 atomic layers.
Has the advantages that: the invention provides an MOCVD device and a method for preparing a two-dimensional crystal material based on ultrasonic atomization, which effectively control the content of a source material passing through an ultrasonic micropore atomization sheet in unit time by adjusting the heating temperature of different sources, the sizes and the number of micropores of the ultrasonic micropore atomization sheet, the vibration frequency, the flow rate of carrier gas of different sources and the flow rate of hydrogen, thereby adjusting the number of the source material adsorbed and deposited on a substrate in unit time, controlling the nucleation and growth speed of the two-dimensional material on the substrate, and adjusting the nucleation density and the grain size of the generated two-dimensional crystal material and the time for forming a continuous single-layer two-dimensional film. The preparation method can obtain discontinuous two-dimensional single crystals by short-time deposition, can obtain continuous single-layer two-dimensional polycrystalline films by long-time growth, and can obtain multilayer two-dimensional crystal films by longer time. The method is simple and easy to implement, solves the problems of poor gas mixing effect and low utilization rate of source materials in the prior art, and is suitable for large-scale production and high-quality preparation of the two-dimensional crystal material with uniform product texture, good repeatability and accurate thickness control.
Drawings
FIG. 1 is a schematic structural view of a first atomizing device used in an embodiment of the present invention;
FIG. 2 is a schematic structural view of a second atomizing device used in the embodiment of the present invention;
FIG. 3 is a schematic structural diagram of an ultrasonic atomizer apparatus used in accordance with an embodiment of the present invention;
FIG. 4 is a three-dimensional view of the structure of an ultrasonic microporous atomizing sheet in an atomizing device employed in an embodiment of the present invention;
FIG. 5 is a schematic diagram illustrating the atomization principle of the ultrasonic microporous atomization sheet in the atomization device adopted in the embodiment of the invention;
FIG. 6 is a schematic diagram of the overall structure of an MOCVD apparatus used in the embodiment of the present invention;
FIG. 7 is a flow chart of a reaction employed in an embodiment of the present invention;
the system comprises a first atomizing device, a second atomizing device, a 3-ultrasonic atomizing nozzle, a 4-reaction chamber, a 11-first atomizing device carrier gas inlet, a 12-first atomizing device cover, a 13-damping rubber, a 14-ultrasonic micropore atomizing sheet, a 15-first atomizing device container, a 16-liquid absorbing cotton, a 17-liquid source, a 21-second atomizing device carrier gas inlet, a 22-second atomizing device cover, a 23-high temperature resistant damping block, a 24-high temperature resistant ultrasonic micropore atomizing sheet, a 25-second atomizing device container, a 26-solid source, a 27-heating base, a 31-gas source inlet, a 32-liquid source steam inlet, a 33-solid source steam inlet, a 34-gas mixing chamber, a 35-gas mixing chamber cover, a 36-high temperature resistant ultrasonic micropore atomizing sheet, a 37-high temperature resistant damping block, a 38-frustum-shaped shield, a 41-piezoelectric ceramic sheet, a 42-conical hole bottom, a 43-metal sheet with conical holes, and a 44-conical hole top.
Detailed Description
The invention will be described in detail below with reference to the following figures and specific embodiments:
as shown in fig. 6, an MOCVD apparatus for preparing a two-dimensional crystal material based on ultrasonic atomization includes:
a gas pipeline for the gaseous source, for direct transmission of the gaseous source;
as shown in fig. 1, a first atomizing device for ultrasonic atomization of a liquid source is used for placing a liquid source material in a first raw material; the first atomization device comprises a container, an ultrasonic micropore atomization sheet, liquid absorption cotton and a cover; the cover is in a step shape, the bottom end of the cover is clamped at the outer side of the top end of the container, an ultrasonic micropore atomization sheet is arranged above the contact part of the cover and the container, damping rubber is arranged between the ultrasonic micropore atomization sheet and the cover, and a carrier gas inlet is arranged on the side surface of the cover above the ultrasonic micropore atomization sheet; an outlet is arranged at the top of the cover; the liquid absorption cotton is positioned in the container, the bottom of the liquid absorption cotton is positioned in the liquid source, and the top of the liquid absorption cotton is connected with the metal sheet of the through hole array on the ultrasonic micropore atomization sheet; the liquid source is transmitted to a metal sheet of a through hole array in the ultrasonic micropore atomization sheet through liquid absorption cotton, and the liquid source is atomized to smaller particles and even vaporized under the drive of piezoelectric ceramics;
as shown in fig. 2, a second atomization device for thermal evaporation ultrasonic atomization of a solid source is used for placing a second raw material, and the second atomization device comprises a container, a high-temperature-resistant ultrasonic micropore atomization sheet and a cover; the cover is in a step shape, the bottom end of the cover is clamped at the outer side of the top end of the container, a high-temperature-resistant ultrasonic micropore atomization sheet is arranged above the contact part of the cover and the container, a high-temperature-resistant damping block is arranged between the high-temperature-resistant ultrasonic micropore atomization sheet and the cover, and a carrier gas inlet is arranged on the side surface of the cover above the high-temperature-resistant ultrasonic micropore atomization sheet; one end of the carrier gas inlet is communicated with the second atomizing device, the other end of the carrier gas inlet is directly communicated with the ultrasonic atomizing nozzle, and the top of the cover is provided with an outlet; the bottom of the container is provided with a heating base, the solid source is placed on the heating base and is heated through a resistance wire at the bottom, so that the solid source is evaporated to a metal sheet of the ultrasonic atomization cone through hole array and is further atomized to smaller particles and even vaporized under the drive of piezoelectric ceramics;
the first atomization device and the second atomization device are modular equipment, and the equipment can be freely combined, such as two first atomization devices can be used for the condition that two sources are both liquid, such as two second atomization devices can be used for the condition that two sources are both solid;
as shown in fig. 3, a reaction chamber device with an ultrasonic atomizer and a sample stage, wherein the ultrasonic atomizer comprises a gas mixing chamber, a high temperature resistant ultrasonic microporous atomizing sheet and a frustum-shaped shield; the top end of the gas mixing chamber is provided with a plurality of gas inlets for connecting the outlets of the gaseous source channel and the non-gaseous source atomization channel, the bottom end of the gas mixing chamber is convexly provided with high-temperature resistant ultrasonic micropore atomization sheets towards two sides, a high-temperature resistant damping block is arranged between the high-temperature resistant ultrasonic micropore atomization sheets and the inner wall of the gas mixing chamber, and the bottom end of the gas mixing chamber is positioned below the high-temperature resistant ultrasonic micropore atomization sheets and is provided with a frustum-shaped shield;
as shown in fig. 4, the ultrasonic microporous atomizing sheet is composed of a high temperature resistant annular piezoelectric ceramic and a metal sheet with a conical hole, wherein one end of the large hole of the conical hole is a liquid inlet hole, the other end of the small hole of the conical hole is a gas outlet hole, the annular piezoelectric ceramic is attached to one surface of the thick hole of the metal sheet, the aperture of the large hole is 5-20 μm, and the aperture of the small hole is 1-5 μm; the driving mode of the ultrasonic micropore atomization sheet is electric field driving, as shown in figure 4, the piezoelectric ceramic and the metal sheet are respectively connected with the anode and the cathode of an alternating current power supply, high-frequency deformation in the vertical direction of the piezoelectric ceramic is caused due to the change of the current direction, so that the metal sheet is driven to vibrate up and down at high frequency, the vertical distance between the small hole of the ultrasonic micropore atomization sheet in the ultrasonic atomization nozzle and the sample table is 5-100 mm, as shown in figure 5, the working principle of the ultrasonic micropore atomization sheet is as follows: when the liquid drops flow from the big holes to the small holes, the flow velocity of the liquid drops is increased, and when the liquid drops flow from the small holes to the big holes, the flow velocity of the liquid drops is decreased, the liquid drops are slowly gathered in the big holes, and after ultrasonic vibration is added, cavitation or micro shock waves are generated to atomize the liquid; when the liquid source reaches the large holes on the metal sheet through the liquid absorption cotton or the solid source reaches the large holes on the metal sheet through evaporation, the piezoelectric ceramic drives the metal sheet to vibrate up and down at the frequency of MHz level, liquid drops and the metal sheet generate rapid relative motion, the liquid source or the solid source of large-particle smog enters the large holes and is rapidly converted into fine-particle smog to be sprayed out, the fine liquid drops are carried to the substrate of the reaction chamber through carrier gas, the thicker liquid drops are generally continuously gasified by a cavitation field generated on the upper surface of the vibrated metal sheet or flow back to accumulate the large holes on the back of the metal sheet, and the liquid drops with certain size are continuously sprayed out from the small holes through ultrasonic cavitation; the sample stage can rotate and be adjusted up and down, and the rotating speed is 100-300 r/min.
The following examples, which include a single solid source, a single liquid source, a single gas source, a combination of a solid source and a liquid source, and a combination of two solid sources, illustrate in detail the method of the present invention for preparing a per-two-dimensional crystalline material:
example 1
Preparing boron alkene on a mica substrate by a chemical vapor deposition method, which comprises the following preparation steps:
(1) Placing a 0.2 mm thick mica substrate on a reaction chamber heating base;
(2) 1 g of NaBH as boron source 4 The powder is placed in a container of a second atomization device;
(3) Pumping the air pressure of the MOCVD system to a limit vacuum state of 0.1 Pa, and keeping for 20 min;
(4) Setting the flow of carrier gas hydrogen connected with the second atomization device to be 10sccm, opening an ultrasonic atomization driver in the second atomization device, and injecting the hydrogen into the reaction chamber;
(5) Raising the temperature of the reaction chamber to 650 ℃, and annealing the mica for 30 min;
(6) The temperature of the second atomization device is raised to 490 ℃ to allow NaBH 4 And decomposing the powder to generate boron source steam, carrying by hydrogen, carrying by ultrasonic refining twice, then reaching the reaction chamber, starting the growth of the boron-alkene two-dimensional atomic crystal, and keeping the temperature for 60 min.
Example 2
Preparing graphene on a quartz substrate by a chemical vapor deposition method, comprising the following preparation steps:
(1) Placing a 4 inch quartz substrate on a reaction chamber heating pedestal;
(2) Placing 100 mL of ethanol in a container of a first atomization device;
(3) Pumping the air pressure of the MOCVD system to a limit vacuum state of 0.1 Pa, and keeping the air pressure for 20 min;
(4) Introducing 20sccm hydrogen into the reaction chamber from the gas path of the gas source to further remove air in the system;
(5) Raising the temperature of the reaction chamber to 1000 ℃, and annealing the quartz substrate for 30 min;
(6) Setting the flow rate of carrier gas hydrogen connected with the first atomization device to be 10sccm, opening an ultrasonic atomization driver in the first atomization device, injecting the hydrogen into the first atomization device, carrying the hydrogen, performing ultrasonic refinement twice, then reaching a reaction chamber, starting growth of graphene two-dimensional atomic crystals, and keeping the temperature for 30 min.
Example 3
Preparing a borolene on a nickel substrate by chemical vapour deposition comprising the following preparation steps:
(1) Placing a nickel foil substrate with the size of 3 x 3 cm on a heating base of a reaction chamber;
(2) Pumping the air pressure of the MOCVD system to a limit vacuum state of 0.1 Pa, and keeping for 20 min;
(3) Introducing 10sccm hydrogen into the reaction chamber from a carrier gas inlet at the side of the second ultrasonic atomizer to further remove air in the system;
(4) Raising the temperature of the reaction chamber to 650 ℃, and annealing the nickel foil substrate for 30 min;
(5) Introducing 10sccm of diborane into the reaction chamber from the gas path of the gas source, reaching the reaction chamber, starting the growth of the boron-alkene two-dimensional atomic crystal, and keeping the temperature for 60 min.
Example 4
By chemical vapour deposition on SiO 2 Preparing molybdenum disulfide on a substrate, comprising the following preparation steps:
(1) Mixing SiO 2 The substrate is arranged on a heating base of the reaction chamber;
(2) Placing diethyl sulfide into a first atomization device container;
(3) Mixing transition metal source Mo (CO) 6 Putting the mixture into a second atomization device container;
(4) Pumping the air pressure of the MOCVD system to a limit vacuum state of 0.1 Pa, and keeping for 20 min;
(5) Heating the second atomization device at 120 ℃ to generate steam, mixing with argon of 10sccm, and introducing into the reaction chamber; simultaneously starting ultrasonic atomization drivers of the first atomization device and the second atomization device, introducing argon of 48sccm into the first atomization device, and introducing a carrier gas carrying source into the reaction chamber;
(6) Introducing hydrogen into the reaction chamber through a gas source gas circuit by 10 sccm;
(7) And heating the sample table to the growth temperature required by the crystals at 620 ℃ to obtain the molybdenum disulfide two-dimensional crystal material.
Example 5
By chemical vapour deposition on SiO 2 The method for preparing indium diselenide on the substrate comprises the following steps:
(1) Mixing SiO 2 The substrate is arranged on a heating base of the reaction chamber;
(2) Pumping the air pressure of the MOCVD system to a limit vacuum state of 0.1 Pa, and keeping the air pressure for 20 min;
(3) Putting selenium powder into a first atomization device, heating to 250 ℃ to generate steam, mixing with 20sccm argon, ultrasonically refining, and introducing into the vacuum chamber;
(4) Meanwhile, indium nitrate is placed into a second atomization device, steam is generated by heating to 250 ℃, argon gas of 20sccm is mixed, and the mixture is subjected to ultrasonic refining and then is introduced into the vacuum chamber;
(5) Adjusting the pressure in the vacuum chamber to 50 Pa;
(6) And heating the sample stage to start the growth of the indium diselenide two-dimensional crystal material.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An MOCVD device for preparing a two-dimensional crystal material based on ultrasonic atomization is characterized by comprising: the device comprises a gas source channel, a non-gaseous source atomization channel, an ultrasonic atomization nozzle and a reaction chamber; the outlet of the gas source channel and the outlet of the non-gaseous source atomizing channel are respectively connected with the inlet of the ultrasonic atomizing nozzle, the outlet of the ultrasonic atomizing nozzle is positioned at the top end of the inner part of the reaction chamber, and the sample stage is arranged at the position under the ultrasonic atomizing nozzle at the bottom end of the inner part of the reaction chamber.
2. The MOCVD device for preparing two-dimensional crystal materials based on ultrasonic atomization, according to claim 1, wherein the non-gaseous source atomization channel is composed of a plurality of liquid source atomization channels, solid source atomization channels or two channels.
3. The MOCVD device for preparing the two-dimensional crystal material based on the ultrasonic atomization, according to claim 2, wherein a liquid source atomization device is arranged in the liquid source atomization channel, and the liquid source atomization device comprises a container, an ultrasonic micropore atomization sheet, liquid absorption cotton and a cover; the cover is in a step shape, the bottom end of the cover is clamped at the outer side of the top end of the container, an ultrasonic micropore atomization sheet is arranged above the contact part of the cover and the container, damping rubber is arranged between the ultrasonic micropore atomization sheet and the cover, and a carrier gas inlet is arranged on the side surface of the cover above the ultrasonic micropore atomization sheet; an outlet is arranged at the top of the cover; the liquid absorption cotton is positioned in the container, the bottom of the liquid absorption cotton is positioned in the liquid source, and the top of the liquid absorption cotton is connected with the metal sheet of the through hole array on the ultrasonic micropore atomization sheet; and a liquid source is transmitted to the metal sheet of the through hole array in the ultrasonic micropore atomization sheet through the liquid absorption cotton, and is atomized to smaller particles and even vaporized under the drive of piezoelectric ceramics.
4. The MOCVD apparatus for preparing two-dimensional crystal material based on ultrasonic atomization as claimed in claim 2, wherein a solid source atomization device is arranged in the solid source atomization channel, and the solid source atomization device comprises a container, a high-ultrasonic-resistance micropore atomization sheet and a cover; the cover is in a step shape, the bottom end of the cover is clamped at the outer side of the top end of the container, a high-temperature-resistant ultrasonic micropore atomization sheet is arranged above the contact part of the cover and the container, a high-temperature-resistant damping block is arranged between the high-temperature-resistant ultrasonic micropore atomization sheet and the cover, and a carrier gas inlet is arranged on the side surface of the cover above the high-temperature-resistant ultrasonic micropore atomization sheet; an outlet is arranged at the top of the cover; the bottom of the container is provided with a heating base, the solid source is placed on the heating base, the solid source is evaporated to a metal sheet of a through hole array in the high-temperature-resistant driver through heating, and the solid source is further atomized to smaller particles and even vaporized under the driving of piezoelectric ceramics.
5. The MOCVD device for preparing the two-dimensional crystal material based on the ultrasonic atomization, according to claim 1, wherein the ultrasonic atomization nozzle comprises a gas mixing chamber, a high-temperature resistant ultrasonic micropore atomization sheet and a frustum-shaped shield; the top of gas mixing chamber sets up a plurality of air inlets for connect gaseous state source passageway and non-gaseous state source atomizing passageway export, the bottom is to the both sides outstanding high temperature resistant supersound micropore atomizing piece of installation, high temperature resistant supersound micropore atomizing piece and mix install high temperature resistant snubber block between the gas mixing chamber inner wall, the gas mixing chamber bottom is located high temperature resistant supersound micropore atomizing piece below and sets up frustum shape guard shield.
6. The MOCVD device for preparing the two-dimensional crystal material based on the ultrasonic atomization as recited in claim 3, 4 or 5, wherein the ultrasonic micropore atomization sheet is composed of high temperature resistant annular piezoelectric ceramics and a metal sheet with a conical hole, a liquid inlet is formed at one end of a large hole of the conical hole, a gas outlet is formed at one end of a small hole of the conical hole, and the annular piezoelectric ceramics is attached to one surface of a large hole of the metal sheet.
7. The MOCVD apparatus for preparing two-dimensional crystal material based on ultrasonic atomization, according to claim 6, wherein the aperture of the big hole at one end is 5-20 μm, and the aperture of the small hole at one end is 1-5 μm.
8. The MOCVD apparatus for preparing two-dimensional crystal material based on ultrasonic atomization as recited in claim 6, wherein a vertical distance between one end of the small hole of the ultrasonic micropore atomization sheet in the ultrasonic atomization nozzle and the sample stage is 5-100 mm.
9. The MOCVD apparatus for preparing two-dimensional crystal material based on ultrasonic atomization, according to claim 1 or 8, wherein the sample stage is rotatable and adjustable up and down.
10. A method for producing a two-dimensional crystalline material using the apparatus of any one of claims 1 to 9, comprising the steps of:
(1) Placing the substrate on a reaction chamber sample stage;
(2) Pumping the gas pressure of the MOCVD device to a limit vacuum state and keeping the gas pressure for 20 min;
(3) Introducing carrier gas into the reaction chamber to further remove air in the system;
(4) Adjusting the temperature and the pressure of the reaction chamber to the temperature and the pressure required by the reaction, and annealing the substrate;
(5) And opening a carrier gas inlet, opening an atomizing device, injecting the refined source material gas into the reaction chamber through the carrier gas, and starting the growth of the two-dimensional crystal material.
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| CN114892270A (en) * | 2022-04-07 | 2022-08-12 | 西安电子科技大学 | Multi-atomization-source Mist-CVD equipment with cold wall time-sharing step-by-step transportation function |
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