Device for two-dimensional material mononuclear nucleation and growth and use method thereof
By designing a single-core nucleation and growth device for two-dimensional materials, the number of crystal nucleation is controlled by baffle through holes, the preparation of large-area single-crystal two-dimensional materials is realized, solving the problem of polycrystalline thin film formation in the prior art and improving the material quality.
Patent Information
- Application Number
- CN202411925008.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-25
- Publication Date
- 2025-04-01
AI Technical Summary
It is difficult to prepare a large-area continuous single-crystal two-dimensional material film. The intra-plane orientation of the crystal nucleation stage in the two-dimensional material nucleation stage leads to the final formation of polycrystals.
A device for single-core nucleation and growth of two-dimensional materials was designed, and the baffle was used to cover the substrate and leave baffle through holes, thereby controlling the number of crystal nucleation in the early stage of growth to achieve single-core nucleation and single-core growth. Growth was performed by expanding baffle through holes to obtain large-area single-crystal two-dimensional material.
The crystal quality of two-dimensional materials has been greatly improved, the preparation of large-area single-crystal two-dimensional materials has been realized, and the formation problem of polycrystalline thin films in the prior art has been solved.
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Figure CN119736712A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of new material technology, and in particular to a device for single-nucleus nucleation and growth of two-dimensional materials and a method of using the device. Background Art
[0002] Two-dimensional materials are a class of materials with unique electronic structures, optical properties and mechanical properties, including transition metal dichalcogenides (TMDs), graphene, black phosphorus, etc. These materials have attracted widespread attention due to their wide application prospects in electronic devices, optoelectronic devices, sensors and other fields. In recent years, researchers have continued to deepen their research on two-dimensional materials, and have made significant progress from the exploration of basic physical properties to the development of practical device applications.
[0003] Take graphene as an example. As the most widely studied and representative two-dimensional material, it has great potential in electronic devices, sensors, energy storage, optoelectronics, etc. due to its excellent electrical conductivity, thermal conductivity, mechanical strength, flexibility and adjustable band gap. For example, graphene can be widely used in high-efficiency batteries, supercapacitors and conductive films. At the same time, its transparency and flexibility make graphene widely used in flexible displays and wearable devices. Boron nitride, as another important two-dimensional material, is often used as an insulating material in electronic devices or as a heat dissipation material in high temperature environments due to its good electrical insulation, thermal conductivity and chemical stability. In addition, the single-layer boron nitride structure can be used in optoelectronics and photocatalysis applications because it can provide efficient light absorption. Molybdenum disulfide, as a typical transition metal disulfide material, has semi-conductive properties and exhibits excellent performance in low-power electronic devices, photodetectors, photocatalysis and other fields. Especially in field effect transistors, MoS2 has become a hot topic of research due to its large carrier mobility and adjustable band gap.
[0004] However, there are still some major challenges to achieve large-scale application of these materials, such as the preparation of high-quality materials, control of large-area uniformity, and compatibility with existing semiconductor processes. The most basic and critical first step is the growth and preparation of large-area high-quality single-crystalline two-dimensional materials. To date, it is very difficult to obtain large-area high-quality single-crystalline films for most two-dimensional materials. For a few typical two-dimensional materials, such as graphene and hexagonal boron nitride, larger single-crystalline films can currently be obtained through metal substrate induction and other methods.
[0005] For most two-dimensional materials, the most widely used method for preparing two-dimensional materials is chemical vapor deposition (CVD), which has unique advantages in the preparation of two-dimensional materials. This method can achieve material growth at a relatively low temperature, which is conducive to deposition on different types of substrates. By precisely controlling parameters such as the flow rate, temperature and pressure of the reaction gas, the growth rate, number of layers and crystal structure of the two-dimensional material can be regulated. CVD technology has been widely used in the preparation of a variety of two-dimensional materials, such as graphene, TMDs (such as MoS2, WS2, etc.), h-BN, etc. Although CVD technology has achieved great success in the preparation of two-dimensional materials, there are still some problems that need to be solved. Although large-area growth can be achieved, at the microscopic scale, there is a certain degree of inhomogeneity in the thickness, composition, crystal structure, and crystallinity of the material. In most cases, polycrystalline thin films are grown, and it is difficult to obtain large-area single-crystalline two-dimensional materials at the wafer level. This will affect the performance of the material and the stability of the device. The control of impurities and defects is also an important issue.
[0006] Molecular beam epitaxy (MBE) can also be used to prepare two-dimensional materials. Since it requires ultra-high vacuum, it faces similar problems as CVD. It is difficult to obtain large-area continuous polycrystalline films. It is even more challenging to use it to prepare large-area single-crystalline two-dimensional material films.
[0007] In summary, there is still a lack of a large-area single crystal thin film growth preparation device and method that is relatively universal for most two-dimensional materials. The core difficulties of large-area continuous single crystal two-dimensional material growth at the wafer level are as follows: the in-plane orientation of the crystal nucleus in the nucleation stage of two-dimensional materials is difficult to be consistent; all materials have fixed crystal structures, and two-dimensional materials have different structures such as triangular, tetragonal, and hexagonal lattices; when two-dimensional materials grow, in the plane parallel to the substrate, the crystal nucleus surrounds the crystal axis perpendicular to the substrate direction, and the lattice orientation is inconsistent; this leads to grain boundaries between the crystal domains when the final growth is completed, and the grain boundaries are difficult to bridge, eventually forming polycrystalline.
[0008] Therefore, the technical methods used in the prior art to prepare two-dimensional materials have the problem of difficulty in preparing large-area continuous single crystal films. Summary of the invention
[0009] The embodiment of the present invention provides a device for single-nucleus nucleation and growth of two-dimensional materials and a method of using the same, aiming to solve the problem that the technical methods used to prepare two-dimensional materials in the prior art are difficult to prepare large-area continuous single crystal films.
[0010] In a first aspect, an embodiment of the present application provides a device for single-nucleus nucleation and growth of two-dimensional materials, wherein the device includes a device housing, a motor, and a motor controller;
[0011] A cavity is provided inside the shell, and an air inlet and an air outlet connected to the cavity are provided at both ends of the shell; a partition is provided at the air inlet to separate the air inlet into a first air inlet cavity and a second air inlet cavity; a first air inlet pipeline and a second air inlet pipeline are connected to the first air inlet cavity and the second air inlet cavity respectively; a rotatable blade is provided at the end of the partition;
[0012] A shell with a semi-enclosed structure is provided in the cavity, and the shell is fixedly connected to the inner wall of the cavity through a support rod; the opening direction of the shell is opposite to the air inlet, and a plurality of baffles are provided on one side of the opening of the shell, and a baffle through hole is formed in the center of the plurality of baffles;
[0013] A substrate tray is provided on one side of the enclosure close to the baffle, and a substrate is mounted in the substrate tray; a heating fixing seat is fixedly provided on the side of the enclosure away from the baffle, and a heating plate is provided between the heating fixing seat and the substrate tray;
[0014] The plurality of motors are arranged on the outer side wall of the shell, and the transmission shafts of the motors are respectively connected to the side edge of one of the baffles; and the motor controllers are respectively electrically connected to the control ends of the motors.
[0015] In a second aspect, an embodiment of the present application further provides a method for using a device for single-nucleus nucleation and growth of a two-dimensional material, wherein the method is applied to the device for single-nucleus nucleation and growth of a two-dimensional material as described in the first aspect above, and the method comprises:
[0016] Sending control instructions to each motor through a motor controller, so as to drive each baffle to move to a central position through the motor, and making the baffle through hole formed by enclosing have a minimum size;
[0017] The heating plate is controlled to heat, and the same or different gases are respectively input into the first air inlet pipeline and the second air inlet pipeline; the two gases are mixed by the rotation of the rotatable blades and nucleated at the baffle through holes to form two-dimensional crystal nuclei; the gas is a metal element gas or a non-metal element gas;
[0018] The motor controller sends a movement instruction to each motor, so that each baffle is driven by the motor to move slowly outward to grow around the two-dimensional crystal core until the entire substrate is completely covered with two-dimensional material.
[0019] In a second aspect, an embodiment of the present application further provides a method for using a device for single-nucleus nucleation and growth of a two-dimensional material, wherein the method is applied to the device for single-nucleus nucleation and growth of a two-dimensional material as described in the first aspect above, and the method comprises:
[0020] Sending control instructions to each motor through a motor controller, so as to drive each baffle to move to a central position through the motor, and making the baffle through hole formed by enclosing have a minimum size;
[0021] Putting a metal solid source or a non-metal solid source into the two solid source crucibles respectively, and heating the air inlet by a heat source so that the two solid source crucibles are in the same or different temperature zones;
[0022] Controlling the heating plate to heat, and using the same or different carrier gases to be respectively input into the first air inlet pipeline and the second air inlet pipeline; rotating the rotatable blades to mix the solid sources carried by the two carrier gases and nucleate at the baffle through holes to form two-dimensional crystal nuclei; the carrier gas is hydrogen or an inert gas;
[0023] The motor controller sends a movement instruction to each motor, so that each baffle is driven by the motor to move slowly outward to grow around the two-dimensional crystal core until the entire substrate is completely covered with two-dimensional material.
[0024] The embodiment of the present invention provides a device for single-nucleus nucleation and growth of two-dimensional materials and a method for using the device, the device includes a device housing, a motor and a motor controller; a cavity is provided inside the housing, and an air inlet and an exhaust port connected to the cavity are provided at both ends of the housing; a partition is provided at the air inlet to separate and form a first air inlet cavity and a second air inlet cavity; a rotatable blade is provided at the end of the partition; a shell with a semi-enclosed structure is provided in the cavity, and the shell is fixedly connected to the inner wall of the cavity through a support rod; the opening direction of the shell is opposite to the air inlet, and a plurality of baffles are provided on one side of the shell opening, and a baffle through hole is formed in the center of the plurality of baffles. The above device uses a baffle to cover the substrate and leaves a baffle through hole, so as to control the number of crystal nuclei in the early stage of growth through the baffle through hole to achieve single-nucleus nucleation and single-nucleus growth, and a large-area single-crystal two-dimensional material is obtained by growing by expanding the baffle through hole, which greatly improves the crystal quality of the two-dimensional material and helps to control and improve the preparation speed of the single-crystal two-dimensional material. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying any creative work.
[0026] Figure 1 A cross-sectional structural diagram of a device for single-nucleus nucleation and growth of two-dimensional materials provided by an embodiment of the present invention;
[0027] Figure 2A side structural diagram of a device for single-nucleus nucleation and growth of two-dimensional materials provided by an embodiment of the present invention;
[0028] Figure 3 Another side structural diagram of the device for single-nucleus nucleation and growth of two-dimensional materials provided by an embodiment of the present invention;
[0029] Figure 4 Another cross-sectional structural diagram of the device for single-nucleus nucleation and growth of two-dimensional materials provided by an embodiment of the present invention;
[0030] Figure 5 Another cross-sectional structural diagram of the device for single-nucleus nucleation and growth of two-dimensional materials provided by an embodiment of the present invention;
[0031] Figure 6 Another cross-sectional structural diagram of the device for single-nucleus nucleation and growth of two-dimensional materials provided by an embodiment of the present invention;
[0032] Figure 7 The following cross-sectional structural diagram of the device for single-nucleus nucleation and growth of two-dimensional materials provided by an embodiment of the present invention;
[0033] Figure 8 A flow chart of a method for using the apparatus for single-nucleus nucleation and growth of two-dimensional materials provided by an embodiment of the present invention;
[0034] Fig. 9 Another flow chart of a method for using the apparatus for single-nucleus nucleation and growth of two-dimensional materials provided in an embodiment of the present invention.
[0035] Figure numerals: 2, device housing; 10, air inlet; 11, first air inlet pipeline; 12, second air inlet pipeline; 13, partition; 14, rotatable blades; 15, solid source crucible; 31, support rod; 32, heating plate; 33, shell; 34, heating fixing seat; 35, substrate; 36, substrate tray; 41, baffle; 42, motor; 43, motor controller; 5, exhaust port. DETAILED DESCRIPTION
[0036] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0037] It should be understood that when used in this specification and the appended claims, the terms "include" and "comprises" indicate the presence of described features, integers, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or combinations thereof.
[0038] It should also be understood that the terms used in the present specification are only for the purpose of describing specific embodiments and are not intended to limit the present invention. As used in the present specification and the appended claims, the singular forms "a", "an" and "the" are intended to include the plural forms unless the context clearly indicates otherwise. It should also be further understood that the term "and / or" used in the present specification and the appended claims refers to any combination of one or more of the associated listed items and all possible combinations, and includes these combinations.
[0039] See also Figure 1 As shown in the figure, a device for single-nucleus nucleation and growth of two-dimensional materials, wherein the device includes a device shell 2, a motor 42 and a motor controller 43; a cavity is provided inside the shell, and an air inlet 10 and an exhaust port 5 connected to the cavity are provided at both ends of the shell; a partition 13 is provided at the air inlet 10 to separate the air inlet 10 to form a first air inlet cavity and a second air inlet cavity; a first air inlet pipeline 11 and a second air inlet pipeline 12 are respectively connected to the first air inlet cavity and the second air inlet cavity; a rotatable blade 14 is provided at the end of the partition 13; a semi-enclosed shell 33 is provided in the cavity, and the shell 33 is fixedly connected to the inner wall of the cavity through a support rod 31 ; The opening direction of the shell 33 is opposite to the air inlet 10, and a plurality of baffles 41 are provided on one side of the opening of the shell 33, and a baffle through hole is formed in the center of the plurality of baffles 41; a substrate tray 36 is provided on the side of the shell 33 close to the baffle 41, and a substrate 35 is assembled in the substrate tray 36; a heating fixing seat 34 is fixedly provided on the side of the shell 33 away from the baffle 41, and a heating plate 32 is provided between the heating fixing seat 34 and the substrate tray 36; a plurality of motors 42 are provided on the outer wall of the shell, and the transmission shafts of the motors 42 are respectively connected to the side of one of the baffles 41; the motor controller 43 is electrically connected to the control end of each motor 42, respectively.
[0040] Specifically, a growth cavity is formed in the enclosure 33. The present application sets a plurality of baffles 41 in the growth cavity of the two-dimensional material and in a position close to the substrate 35 directly in front of the substrate 35. The bottom partition of the substrate 35 is blocked by a plurality of movable baffles 41 combined at a specific angle, and the size of the baffle through hole (the uncovered area in the middle of the baffle 41) is adjusted by controlling the movement of the baffle 41, thereby controlling the number of nuclei of the two-dimensional material and achieving single-nuclei nucleation. The present application provides a device and a method for use that realizes single-nuclei nucleation of two-dimensional materials and can perform single-nuclei growth of large-area single-crystal two-dimensional materials, providing a new effective liberation solution for the future industrial preparation of large-area single-crystal two-dimensional materials and new devices, and this solution is generally applicable to almost all two-dimensional materials. Among them, the distance between the baffle 41 and the substrate 35 can be set to be no more than 1 mm, the smaller the spacing between the substrate 35 and the baffle 41, the better, and the baffles 41 are parallel and close to each other.
[0041] The motor controller 43 is connected to the multiple motors 42 through multiple control paths, and each baffle 41 is connected to the transmission shaft of a motor 42. Specifically, the baffle 41 and the motor 42 are connected by a mechanical arm, and the outside of the mechanical arm is sealed by a retractable bellows sleeve; the motor 42 can be synchronously controlled through multiple control paths, so as to control the baffle 41 to move outward from the center of the substrate 35 at the same or different speeds. The start and stop and speed of all motors 42 are controlled by a motor controller 43, and all motors 42 can rotate at the same or different speeds.
[0042] In the structure of the above-mentioned device, the number of baffles 41 and the angle between adjacent baffles 41 are determined by the lattice structure of the two-dimensional material. The number n of baffles 41 is the same as the number N of side lengths of the lattice in the unit cell of the two-dimensional material, that is, n=N. Among them, the angle between adjacent baffles 41 is the same as the angle between adjacent sides of the lattice in the unit cell of the two-dimensional material. Each baffle 41 is evenly arranged around the center of the substrate 35, and all baffles 41 are combined to form a baffle through hole of any size not covered by the baffle 41 with the center of the substrate 35 as the center. The size of the baffle through hole can be adjusted arbitrarily within the range from nanometer level to covering the entire substrate 35, and the shape of the baffle through hole is consistent with the in-plane lattice shape of the unit cell of the two-dimensional material.
[0043] The two gases input by the first gas inlet pipeline 11 and the second gas inlet pipeline 12 can be metal element gas sources or non-metal element gas sources, or carrier gases. If both gases are carrier gases, which can be hydrogen or inert gases, a solid source crucible 15 can be provided in the first gas inlet cavity and the second gas inlet cavity, and the carrier gas passes through the solid source crucible 15 to form a gas carrying a solid source for crystal growth. The specific device structure is as follows: Figure 4 shown.
[0044] The motor 42 is a stepper motor 42 or other type of motor 42. The motor 42 must be a high-precision motor 42. The minimum precision of the motor 42 moving step length control can be as low as 10 nanometers, which means that the control of the moving step length of 10 nanometers and above can be achieved (the smaller the controllable moving step length, the better). The moving speed of the baffle 41 controlled by the motor 42 is adjustable, and the adjustable range is greater than 1 micron / second to 1 mm / second, which matches the lateral growth rate of the two-dimensional material.
[0045] In a more specific embodiment, the ventilation directions of the first air inlet pipeline 11 and the second air inlet pipeline 12 are parallel or axially symmetrical, and the baffle 41, the substrate tray 36, and the heating plate 32 are arranged in parallel in sequence. Among them, the baffle 41 is perpendicular to the central axis of the first air inlet pipeline 11 and the second ventilation pipeline. Specifically, the partition 13 is perpendicular to the baffle 41, and the distance between the partition 13 and the baffle 41 is not greater than 15 cm.
[0046] In order to improve the quality of crystal growth, the ventilation directions of the first air inlet pipeline 11 and the second air inlet pipeline 12 can be set to be parallel, such as Figure 1 , Figure 4 , Figure 5 and Figure 6 As shown, the two gases are input in parallel and mixed at the rotatable blade 14. Since the two gases move in the axial direction, the rotatable blade 14 can be driven to rotate by the airflow, and the rotation of the rotatable blade 14 generates a rotational force and mixes the two gases. A baffle 41, a substrate tray 36 and a heating plate 32 can also be arranged in parallel in sequence, and the substrate 35 arranged in the substrate tray 36 is also parallel to the baffle 41, so that the substrate 35 can evenly receive the blown gas, and the heating plate 32 can evenly heat the substrate 35, so that the crystal growth is more uniform and the quality of the obtained two-dimensional material is improved.
[0047] The ventilation directions of the first air intake pipeline 11 and the second air intake pipeline 12 may also be symmetrically arranged. The specific structure is as follows: Figure 7 shown.
[0048] Furthermore, each baffle 41 can be arranged perpendicular to the central axis of the first air inlet pipeline 11 and the second air inlet pipeline 12, so that the baffle through hole can accurately receive the input mixed gas, and the inflow direction of the mixed gas is perpendicular to the setting direction of the baffle 41. In order to allow the two gases to mix only when they enter a position close to the baffle 41, the spacing between the baffle 13 and the baffle 41 can be set to be no more than 15 cm, thereby minimizing pre-reaction and improving the quality of the two-dimensional material. If used to produce single-element two-dimensional materials, the baffle 13 is not required, and the precursor gas and the carrier gas can be directly mixed.
[0049] In a more specific embodiment, the ventilation directions of the first air intake pipeline 11 and the second air intake pipeline 12 are both horizontal, or the ventilation directions of the first air intake pipeline 11 and the second air intake pipeline 12 are both vertical.
[0050] The ventilation direction can be horizontal or vertical. For example, Figure 1 and Figure 4 As shown, the ventilation direction is vertical. Figure 5 and Figure 6 As shown. If the input gas is a metal element gas source or a non-metal element gas source, then the gas source is used as the crystal growth source in the input device; if the input gas is a carrier gas carrying a solid source, then the gas source is used as the crystal growth source in the input device. More specifically, the deposition gas pressure for crystal growth can be normal pressure, low pressure or ultra-high vacuum, among which the effect of single-nucleus nucleation and single-nucleus growth in ultra-high vacuum is the best.
[0051] The baffle 41 in front of the substrate 35 is pushed toward the center of the substrate 35 before the two-dimensional material grows, until it is near the center of the substrate 35, but does not completely cover the substrate 35, exposing a polygonal baffle through hole with a side length of micrometers; the shape of the baffle through hole is consistent with the lattice shape of the two-dimensional material unit cell. Since the nucleation size of the two-dimensional material is generally in the order of submicrometer to tens of micrometers, the size of the baffle through hole should be slightly smaller than the size of a single crystal nucleus to control the growth of a single nucleus.
[0052] In a more specific embodiment, three baffles 41 are disposed at the opening of the enclosure 33 , and the three baffles 41 enclose and form an equilateral triangle baffle through hole.
[0053] Specifically, in one embodiment, when the unit cell lattice of the grown two-dimensional material is an equilateral triangle lattice, three baffles 41 may be provided, and the three baffles 41 may enclose an equilateral triangle baffle through hole, such as Figure 2 As shown; the angle between adjacent baffles 41 is 120 degrees. Before the growth begins, the three baffles 41 form an equilateral triangle baffle hole near the center of the substrate 35, and the side length of the baffle hole is 10 nanometers. The two-dimensional material precursor forms a single crystal nucleus only at the equilateral triangle baffle hole. Then, under the control of the high-precision motor 42, the three baffles 41 move outward at a certain speed with the center of the substrate 35 as the symmetry center. The movement rate is less than or equal to the lateral growth rate of the two-dimensional material on this substrate 35, and the growth boundary is consistently maintained at the inner edge of the baffle 41 until the entire substrate 35 is completely covered with single-crystalline two-dimensional material.
[0054] The reaction precursor is supplied by a gas source. For compound two-dimensional materials, the gas inlet path is divided into metal elements and non-metal elements, and the two gases are mixed with carrier gases (such as hydrogen) respectively; when the two gases are respectively delivered to the front of the substrate 35, the rotating blades 14 are used to rotate and mix them, and the growth is carried out at a pressure of 200mbar. The ventilation direction of the gas inlet pipeline is horizontal or vertical, and the specific application is as follows Figure 1 , Figure 5 and Figure 6 shown.
[0055] In another embodiment, four baffles 41 are disposed at the opening of the enclosure 33 , and the four baffles 41 enclose and form a square baffle through hole.
[0056] When the unit cell lattice of the grown two-dimensional material is a cubic lattice, the number of baffles 41 in front of the substrate 35 is set to four, and the angle between adjacent baffles 41 is 90 degrees. The specific setting structure is as follows: Figure 3 As shown. Before the growth begins, four baffles 41 form a square baffle through hole near the center of the substrate 35, and the side length of the baffle through hole is 10 nanometers. The two-dimensional material precursor forms a single crystal nucleus only at the baffle through hole, and then the four baffles 41, under the control of the high-precision motor 42, move outward at a certain speed with the center of the substrate 35 as the symmetry center. The movement rate is less than or equal to the lateral growth rate of the two-dimensional material on this substrate 35, and the growth boundary is consistently maintained at the inner edge of the baffle 41 until the entire substrate 35 is completely covered with single-crystalline two-dimensional material.
[0057] This two-dimensional material is a compound, and the metal elements and non-metal elements are both solid sources, which are separated. At this time, a solid source crucible 15 needs to be set in the first air inlet cavity and the second air inlet cavity, and the solid source crucible 15 is placed in different heating temperature zones and transported by a carrier gas (hydrogen or inert gas). When the solid source is transported to the front of the substrate 35 by the carrier gas, it is rotated and mixed by the rotating rotatable blades 14, and grown at a pressure of 10Pa. The ventilation direction of the air inlet pipeline is horizontal, such as Figure 4 shown.
[0058] Alternatively, six baffles 41 are disposed at the opening of the enclosure 33 , and the six baffles 41 enclose a regular hexagonal baffle through hole.
[0059] When the unit cell lattice of the growing two-dimensional material is a hexagonal lattice, there are six baffles 41 in front of the substrate 35, and the angle between adjacent baffles 41 is 60 degrees. Before the growth begins, the six baffles 41 form a regular hexagonal baffle hole near the center of the substrate 35, and the side length of the regular hexagonal baffle hole is 50 nanometers. The two-dimensional material precursor forms only a single crystal nucleus at the baffle hole. Subsequently, the six baffles 41, under the control of a high-precision motor 42, move outward at a certain rate with the center of the substrate 35 as the symmetry center. The movement rate is less than or equal to the lateral growth rate of the two-dimensional material on this substrate 35, and the growth boundary is consistently maintained at the inner edge of the baffle 41 until the entire substrate 35 is completely covered with single-crystalline two-dimensional material. The growth object is a compound two-dimensional material, there are multiple solid sources, and the background vacuum of the growth environment is 2×10 -8 Pa (ultra-high vacuum), the heat source is thermal evaporation or electron beam evaporation jet furnace, the specific structure is as follows Figure 7 shown.
[0060] The above-mentioned setting structure is only an example for illustration. The scheme can be implemented with three baffles, four baffles and six baffles. In other embodiments, more or fewer baffles can be used to form baffle holes of other shapes, such as eight baffles combined to form a regular octagonal baffle hole.
[0061] The present invention also provides a method for using the device for single-nucleus nucleation and growth of two-dimensional materials. The method is applied to the device for single-nucleus nucleation and growth of two-dimensional materials described in the above embodiment, such as Figure 8 As shown, the method includes steps S11-S13.
[0062] S11, sending a control instruction to each motor through a motor controller, so as to drive each baffle to move to a central position through the motor, and make the baffle through hole formed by enclosing have a minimum size.
[0063] First, a control instruction can be issued through the motor controller to control the baffle to move to the center position, at which time the baffle through hole formed by the baffle has a minimum size.
[0064] S12, controlling the heating plate to heat, and using the same or different gases to be input into the first air inlet pipeline and the second air inlet pipeline respectively; the two gases are mixed by rotating the rotatable blades and nucleated at the baffle holes to form two-dimensional crystal nuclei; the gas is a metal element gas or a non-metal element gas.
[0065] The heating plate is controlled to heat, and the same or different gases are respectively input into the first air inlet pipeline and the second air inlet pipeline. The gases input into the first air inlet pipeline and the second air inlet pipeline can be both metal element gases or non-metal element gases, or the first air inlet pipeline can be a metal element gas source and the second air inlet pipeline can be a non-metal element gas. In this case, there is no need to set a solid source crucible in the first air inlet cavity and the second air inlet cavity.
[0066] S13, sending a movement instruction to each motor through the motor controller, so as to drive each baffle to move slowly outward through the motor, so as to grow around the two-dimensional crystal core until the entire substrate is completely covered with two-dimensional material.
[0067] Further, a movement instruction is sent to each motor through the motor controller, so that the baffle is driven by the motor to move slowly outward, and the movement rate of the baffle is less than or equal to the lateral growth rate of the two-dimensional material on this substrate.
[0068] The present invention also provides a method for using the device for single-nucleus nucleation and growth of two-dimensional materials. The method is applied to the device for single-nucleus nucleation and growth of two-dimensional materials described in the above embodiment, such as Fig. 9 As shown, the method includes steps S21-S24.
[0069] S21, sending a control instruction to each motor through a motor controller, so as to drive each baffle to move to a central position through the motor, and make the baffle through hole formed by enclosing have a minimum size.
[0070] S22. Put a metal solid source or a non-metal solid source into the two solid source crucibles respectively, and heat the air inlet by a heat source so that the two solid source crucibles are in the same or different temperature zones.
[0071] Solid source crucibles can be respectively arranged in the first air inlet cavity and the second air inlet cavity, and the air inlet can be heated by a heat source to adjust the placement of the solid source crucibles, so that the two solid source crucibles are in the same or different temperature zones.
[0072] S23, controlling the heating plate to heat, and using the same or different carrier gases to be input into the first air inlet pipeline and the second air inlet pipeline respectively; the rotatable blades are rotated to mix the solid sources carried by the two carrier gases and nucleate at the baffle holes to form two-dimensional crystal nuclei; the carrier gas is hydrogen or an inert gas.
[0073] The heating plate is controlled to heat, and the same or different carrier gases are used to input into the first air inlet pipeline and the second air inlet pipeline respectively. For example, the carrier gases input into the first air inlet pipeline and the second air inlet pipeline can both be hydrogen, or one carrier gas can be hydrogen and the other gas can be an inert gas (argon, helium, etc.).
[0074] S24, sending a movement instruction to each motor through the motor controller, so as to drive each baffle to move slowly outward through the motor, so as to grow around the two-dimensional crystal core until the entire substrate is completely covered with two-dimensional material.
[0075] The embodiment of the present invention provides a device for single-nucleus nucleation and growth of two-dimensional materials and a method for using the device, the device includes a device housing, a motor and a motor controller; a cavity is provided inside the housing, and an air inlet and an exhaust port connected to the cavity are provided at both ends of the housing; a partition is provided at the air inlet to separate and form a first air inlet cavity and a second air inlet cavity; a rotatable blade is provided at the end of the partition; a shell with a semi-enclosed structure is provided in the cavity, and the shell is fixedly connected to the inner wall of the cavity through a support rod; the opening direction of the shell is opposite to the air inlet, and a plurality of baffles are provided on one side of the shell opening, and a baffle through hole is formed in the center of the plurality of baffles. The above device uses a baffle to cover the substrate and leaves a baffle through hole, so as to control the number of crystal nuclei in the early stage of growth through the baffle through hole to achieve single-nucleus nucleation and single-nucleus growth, and a large-area single crystal two-dimensional material is obtained by growing by expanding the baffle through hole, which greatly improves the growth rate and quality of the two-dimensional material.
[0076] The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can easily think of various equivalent modifications or replacements within the technical scope disclosed by the present invention, and these modifications or replacements should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention shall be based on the protection scope of the claims.
Claims
1. A device for single-nucleus nucleation and growth of two-dimensional materials, characterized in that: The device comprises a device housing, a motor and a motor controller; A cavity is provided inside the shell, and an air inlet and an air outlet connected to the cavity are provided at both ends of the shell; a partition is provided at the air inlet to separate the air inlet into a first air inlet cavity and a second air inlet cavity; a first air inlet pipeline and a second air inlet pipeline are connected to the first air inlet cavity and the second air inlet cavity respectively; a rotatable blade is provided at the end of the partition; A shell with a semi-enclosed structure is provided in the cavity, and the shell is fixedly connected to the inner wall of the cavity through a support rod; the opening direction of the shell is opposite to the air inlet, and a plurality of baffles are provided on one side of the opening of the shell, and a baffle through hole is formed in the center of the plurality of baffles; A substrate tray is provided on one side of the enclosure close to the baffle, and a substrate is mounted in the substrate tray; a heating fixing seat is fixedly provided on the side of the enclosure away from the baffle, and a heating plate is provided between the heating fixing seat and the substrate tray; The plurality of motors are arranged on the outer side wall of the shell, and the transmission shafts of the motors are respectively connected to the side edge of one of the baffles; and the motor controllers are respectively electrically connected to the control ends of the motors.
2. The device for single-nucleus nucleation and growth of two-dimensional materials according to claim 1, characterized in that: The ventilation directions of the first air inlet pipeline and the second air inlet pipeline are parallel or axially symmetrically arranged, and the baffle, the substrate tray, and the heating plate are sequentially arranged in parallel.
3. The device for single-nucleus nucleation and growth of two-dimensional materials according to claim 2, characterized in that: The baffles are perpendicular to the central axes of the first air intake pipeline and the second air ventilation pipeline.
4. The device for single-nucleus nucleation and growth of two-dimensional materials according to claim 3, characterized in that: The partition is perpendicular to the baffle, and the distance between the partition and the baffle is no more than 15 cm.
5. The device for single-nucleus nucleation and growth of two-dimensional materials according to claim 4, characterized in that: The ventilation directions of the first air intake pipeline and the second air intake pipeline are both vertical directions, or the ventilation directions of the first air intake pipeline and the second air intake pipeline are both horizontal directions.
6. The device for single-nucleus nucleation and growth of two-dimensional materials according to any one of claims 1 to 5, characterized in that: Three baffles are arranged at the opening of the enclosure, and the three baffles enclose an equilateral triangle baffle through hole.
7. The device for single-nucleus nucleation and growth of two-dimensional materials according to any one of claims 1 to 5, characterized in that: Four baffles are arranged at the opening of the enclosure, and the four baffles are enclosed to form a square baffle through hole.
8. The device for single-nucleus nucleation and growth of two-dimensional materials according to any one of claims 1 to 5, characterized in that: Six baffles are arranged at the opening of the enclosure, and the six baffles are combined to form a regular hexagonal baffle through hole.
9. A method for using a device for single-nucleus nucleation and growth of two-dimensional materials, characterized in that: The method of use is applied to the device for single-nucleus nucleation and growth of two-dimensional materials as claimed in any one of claims 1 to 8, and the method comprises: Sending control instructions to each motor through a motor controller, so as to drive each baffle to move to a central position through the motor, and making the baffle through hole formed by enclosing have a minimum size; The heating plate is controlled to heat, and the same or different gases are respectively input into the first air inlet pipeline and the second air inlet pipeline; the two gases are mixed by the rotation of the rotatable blades and nucleated at the baffle through holes to form two-dimensional crystal nuclei; the gas is a metal element gas or a non-metal element gas; The motor controller sends a movement instruction to each motor, so that each baffle is driven by the motor to move slowly outward to grow around the two-dimensional crystal core until the entire substrate is completely covered with two-dimensional material.
10. A method for using a device for single-nucleus nucleation and growth of two-dimensional materials, characterized in that: The method of use is applied to the device for single-nucleus nucleation and growth of two-dimensional materials as claimed in any one of claims 1 to 8, and the method comprises: Sending control instructions to each motor through a motor controller, so as to drive each baffle to move to a central position through the motor, and making the baffle through hole formed by enclosing have a minimum size; Putting a metal solid source or a non-metal solid source into the two solid source crucibles respectively, and heating the air inlet by a heat source so that the two solid source crucibles are in the same or different temperature zones; Controlling the heating plate to heat, and using the same or different carrier gases to be respectively input into the first air inlet pipeline and the second air inlet pipeline; rotating the rotatable blades to mix the solid sources carried by the two carrier gases and nucleate at the baffle through holes to form two-dimensional crystal nuclei; the carrier gas is hydrogen or an inert gas; The motor controller sends a movement instruction to each motor, so that each baffle is driven by the motor to move slowly outward to grow around the two-dimensional crystal core until the entire substrate is completely covered with two-dimensional material.