CN116988148A - Preparation method of two-dimensional beta-gallium oxide crystal film - Google Patents
Preparation method of two-dimensional beta-gallium oxide crystal film Download PDFInfo
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- CN116988148A CN116988148A CN202311045476.2A CN202311045476A CN116988148A CN 116988148 A CN116988148 A CN 116988148A CN 202311045476 A CN202311045476 A CN 202311045476A CN 116988148 A CN116988148 A CN 116988148A
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- 239000013078 crystal Substances 0.000 title claims abstract description 84
- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 49
- 239000000758 substrate Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 43
- 238000001451 molecular beam epitaxy Methods 0.000 claims abstract description 27
- 229910052760 oxygen Inorganic materials 0.000 claims description 42
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 41
- 239000001301 oxygen Substances 0.000 claims description 41
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 35
- 229910052733 gallium Inorganic materials 0.000 claims description 23
- 238000000197 pyrolysis Methods 0.000 claims description 11
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 description 34
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 9
- 239000010409 thin film Substances 0.000 description 9
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 238000001636 atomic emission spectroscopy Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 238000000407 epitaxy Methods 0.000 description 3
- 238000001657 homoepitaxy Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 229910001338 liquidmetal Inorganic materials 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000002128 reflection high energy electron diffraction Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire 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
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000000927 vapour-phase epitaxy Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/025—Epitaxial-layer growth characterised by the substrate
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/005—Oxydation
Abstract
The application discloses a preparation method of a two-dimensional beta-gallium oxide crystal film, which comprises the following steps: s1, providing a beta-gallium oxide single crystal substrate; s2, covering a van der Waals material layer on the beta-gallium oxide single crystal substrate; and S3, epitaxially growing a two-dimensional beta-gallium oxide crystal film on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer by adopting a molecular beam epitaxy process. According to the application, the homogeneous substrate is covered with the van der Waals material layer, and the high-quality two-dimensional beta-gallium oxide crystal film can be epitaxially grown on the van der Waals material layer by adopting a molecular beam epitaxy process, so that the method can be widely applied to power electronic devices, intelligent wearing and high-density batteries.
Description
Technical Field
The application belongs to the technical field of semiconductors, and particularly relates to a preparation method of a two-dimensional beta-gallium oxide crystal film.
Background
Gallium oxide (Ga) 2 O 3 ) Is thatA wide bandgap semiconductor material comprising alpha, beta, gamma, delta and epsilon phases, wherein beta-Ga 2 O 3 (beta-phase Ga 2 O 3 ) Is the most stable form, beta-Ga 2 O 3 Has many excellent electrical and optical properties with a band gap of 4.9eV, and thus has attracted extensive attention and research in the field of semiconductor devices.
β-Ga 2 O 3 As a novel semiconductor material, the semiconductor material has the potential of breaking through the traditional semiconductor technology, can provide higher power density and higher working temperature for the existing electronic device, and has high breakdown electric field strength of gallium oxide, so that the gallium oxide becomes an ideal candidate material in the power electronic device, such as a power switch, power supply electronics, a photovoltaic inverter and the like. Gallium oxide also has potential applications in photovoltaic devices, such as ultraviolet photodetectors, deep ultraviolet light emitters, and the like, due to its wide bandgap characteristics. Currently, beta-Ga 2 O 3 The crystal film is mainly prepared by chemical vapor deposition, halide vapor phase epitaxy, molecular beam epitaxy and magnetron sputtering, and beta-Ga 2 O 3 The crystal film has larger lattice mismatch with the conventional silicon, sapphire and other heterogeneous substrates, and the quality of the prepared single crystal film is not excellent. While concerning beta-Ga 2 O 3 Less research on crystal film and high-quality two-dimensional beta-Ga 2 O 3 The crystal film can be applied to power electronic devices, intelligent wearing and high-density batteries. Currently, it is taught by Shandong university Qian Kai to prepare smooth, continuous, uniform Ga by liquid metal extrusion blotting 2 O 3 The thickness of the film is about 3 nm.
In the prior art, two-dimensional beta-Ga is prepared by a liquid metal extrusion imprinting method 2 O 3 Amorphous state, and poor film quality, and cannot be truly and effectively utilized in the structural layers of the device. The film grown by chemical vapor deposition and halide vapor epitaxy deposition has poor crystallinity and cannot precisely control the number of grown layers, and is mainly used for growing beta-Ga 2 O 3 And (3) single crystals. Magnetron sputtering generally can only grow polycrystalline or amorphous beta-Ga with poor crystallinity 2 O 3 . MoleculesIn current homogeneous or heterogeneous epitaxy, the beam epitaxy apparatus causes a buffer layer that is amorphous during the first 5 layers of growth due to the lower mobility of Ga on the nonmetallic substrate, the growth mode is island growth, then islands merge, and then gradually grow in a lamellar mode.
Therefore, in view of the above technical problems, it is necessary to provide a method for preparing a two-dimensional β -gallium oxide crystal thin film.
Disclosure of Invention
In view of the above, the present application aims to provide a method for preparing a two-dimensional β -gallium oxide crystal thin film.
In order to achieve the above object, an embodiment of the present application provides the following technical solution:
a method for preparing a two-dimensional beta-gallium oxide crystal film, comprising the following steps:
s1, providing a beta-gallium oxide single crystal substrate;
s2, covering a van der Waals material layer on the beta-gallium oxide single crystal substrate;
and S3, epitaxially growing a two-dimensional beta-gallium oxide crystal film on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer by adopting a molecular beam epitaxy process.
In one embodiment, the van der waals material layer is a graphene layer or a hexagonal boron nitride layer, and the thickness is 1-3 atomic layers.
In one embodiment, the thickness of the van der Waals material layer is 0.2nm to 2nm.
In one embodiment, the step S3 includes:
providing a molecular beam epitaxy system having a gallium source and an oxygen source;
placing the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer on a growth table in a molecular beam epitaxy system, heating a gallium source to provide gallium atoms, closing an oxygen source, and growing a gallium layer on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer;
and opening an oxygen source to provide oxygen, performing radio frequency pyrolysis on the oxygen, and reacting oxygen atoms after the radio frequency pyrolysis with gallium atoms in an oxygen-enriched atmosphere to grow to obtain the two-dimensional beta-gallium oxide crystal film.
In one embodiment, the heating temperature of the gallium source is 800-1100 ℃, and the flow rate of the gallium source isAnd/or the number of the groups of groups,
the oxygen flow provided by the oxygen source is 0.5 sccm-5 sccm; and/or the number of the groups of groups,
the power of the oxygen radio frequency pyrolysis is 200W-350W; and/or the number of the groups of groups,
the reaction time of the oxygen atoms and the gallium atoms is 30 min-300 min.
In one embodiment, the molecular beam epitaxy process is performed under vacuum at a pressure of 10 -7 Torr～10- 10 Torr。
In one embodiment, the temperature of the growth stage in the molecular beam epitaxy system is 250 ℃ to 350 ℃ prior to opening the oxygen source; after the oxygen source is turned on, the temperature of a growth table in the molecular beam epitaxy system is 500-600 ℃.
In an embodiment, the step S2 further includes:
and (3) carrying out an annealing process on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer under the vacuum condition, wherein the annealing temperature is 200-400 ℃, and the annealing time is 3-24 h.
In an embodiment, the step S3 further includes:
and cooling the grown two-dimensional beta-gallium oxide crystal film at a cooling rate of 1-30K/min.
In an embodiment, the step S3 further includes:
and stripping the grown two-dimensional beta-gallium oxide crystal film from the beta-gallium oxide single crystal substrate through a mechanical stripping process or an ultrasonic stripping process.
The application has the following beneficial effects:
according to the application, the homogeneous substrate is covered with the van der Waals material layer, and the high-quality two-dimensional beta-gallium oxide crystal film can be epitaxially grown on the van der Waals material layer by adopting a molecular beam epitaxy process, so that the method can be widely applied to power electronic devices, intelligent wearing and high-density batteries.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings may be obtained according to the drawings without inventive effort to those skilled in the art.
FIG. 1 is a schematic flow chart of a method for preparing a two-dimensional beta-gallium oxide crystal film according to the application;
FIG. 2 is an SEM image of a two-dimensional beta-gallium oxide crystal film according to an embodiment of the application;
FIG. 3 is an AFM image of a two-dimensional beta-gallium oxide crystal film according to an embodiment of the application;
fig. 4 is an SEM image and an AES image of a two-dimensional β -gallium oxide crystal thin film according to an embodiment of the present application.
Detailed Description
In order to make the technical solution of the present application better understood by those skilled in the art, the technical solution of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present application without making any inventive effort, shall fall within the scope of the present application.
Referring to fig. 1, the application discloses a preparation method of a two-dimensional beta-gallium oxide crystal film, which comprises the following steps:
s1, providing a beta-gallium oxide single crystal substrate;
s2, covering a van der Waals material layer on the beta-gallium oxide single crystal substrate;
and S3, epitaxially growing a two-dimensional beta-gallium oxide crystal film on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer by adopting a molecular beam epitaxy process.
The application prepares the two-dimensional beta-gallium oxide crystal film based on the van der Waals epitaxial process of the homogeneous substrate by utilizing the molecular beam epitaxy equipment, the substrate adopts the beta-gallium oxide single crystal substrate, and a van der Waals material layer is covered on the substrate, so that the two-dimensional beta-gallium oxide crystal film with the transverse dimension in the micron level can be obtained by growth.
The application is further illustrated below with reference to specific examples.
In one embodiment of the present application, the method for preparing a two-dimensional β -gallium oxide crystal thin film comprises the steps of:
1. a beta-gallium oxide single crystal substrate is provided.
The substrate in this embodiment is a homogeneous substrate, i.e., a β -gallium oxide single crystal substrate.
The advantages of using a homogeneous substrate over a heterogeneous substrate are:
1. lattice matching and quality control:
the homoepitaxy enables the lattice matching degree of the film and the substrate to be higher, and is helpful for reducing defects and stress caused by lattice mismatch, which is helpful for improving the crystallization quality and electrical property of the film;
2. material purity and consistency:
in homoepitaxial growth, the substrate and the grown film are both the same material, which helps to ensure consistency and purity of the material, which is important for repeatability and stability in research and device manufacturing processes;
3. material study and performance optimization:
through homoepitaxy, the performance and the growth mechanism of the gallium oxide material and the relation between the material and the device can be better explored, which is helpful for optimizing the performance of the gallium oxide material and is more suitable for different applications;
4. interface defects are reduced:
the homoepitaxy growth can reduce defects caused by interfaces in the epitaxial growth process, and improve the performance and stability of the device.
2. And covering a van der Waals material layer on the beta-gallium oxide single crystal substrate.
The van der Waals material layer in the application can be a graphene layer or a hexagonal boron nitride layer (h-BN), and the thickness of the van der Waals material layer is 1-3 atomic layers, and the corresponding thickness is about 0.2-2 nm.
Illustratively, in this embodiment, a graphene layer is selected as the van der waals material layer, and the thickness is 3 atomic layers, which corresponds to a thickness of about 1nm.
According to the application, a van der Waals material layer with the thickness of 1-3 atomic layers is selected, and van der Waals epitaxial growth is carried out on a homogeneous substrate, and the advantage is that:
1. reducing lattice mismatch defects:
van der waals epitaxial growth avoids the defect problem caused by lattice mismatch in conventional epitaxial growth, because in this technique, the growth of the thin film is independent of the lattice of the base material;
2. lattice matching:
one of the advantages of van der waals epitaxial growth is that it does not rely on lattice matching, as the material grown may have different lattice parameters;
3. lattice constant modulation:
of the van der waals materials of layers 1-3, the crystal lattice of the lowermost support substrate also modulates the lattice constant of the film grown thereon.
3. And epitaxially growing a two-dimensional beta-gallium oxide crystal film on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer by adopting a molecular beam epitaxy process.
First, a molecular beam epitaxy system having a gallium source and an oxygen source is provided.
Illustratively, the purity of the gallium source in this example is not less than 99.999% and the purity of the oxygen source is not less than 99.999%. The gallium source and the oxygen source are installed in the molecular beam epitaxy system, and ensure that they can be controlled by an electron beam thermal evaporation source, a gas radio frequency cracking source, and ensure that the whole system can realize a high vacuum environment (about 10 -7 Torr～10 -10 Torr)。
Further, before epitaxial growth, the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer is annealed under vacuum condition at 200-400 ℃ for 3-24 h. The annealing time length is determined according to the vacuum degree, and the vacuum degree can be stopped without changing, and preferably, the annealing temperature in the embodiment is 300 ℃ and the annealing time is 3 hours.
Then, the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer is placed on a growth stage in a molecular beam epitaxy system, a gallium source is heated to provide gallium atoms, an oxygen source is closed, and a gallium layer is grown on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer.
And finally, opening an oxygen source to provide oxygen, performing radio frequency pyrolysis on the oxygen, and reacting oxygen atoms after the radio frequency pyrolysis with gallium atoms in an oxygen-enriched atmosphere to grow to obtain the two-dimensional beta-gallium oxide crystal film.
In this embodiment, the heating temperature of the gallium source is 800-1100 ℃, and the flow rate of the gallium source isThe flow rate of oxygen provided by the oxygen source is 0.5 sccm-5 sccm; the power of the oxygen radio frequency pyrolysis is 200W-350W; the reaction time of oxygen atoms and gallium atoms is 30 min-300 min; the molecular beam epitaxy process is carried out under vacuum condition with pressure of 10 -7 Torr～10 -10 Torr；
In addition, before the oxygen source is opened, the temperature of a growth table in the molecular beam epitaxy system is 250-350 ℃; after the oxygen source is turned on, the temperature of a growth table in the molecular beam epitaxy system is 500-600 ℃.
Illustratively, the growth process in this embodiment is specifically as follows:
placing the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer on a growth table in a molecular beam epitaxy system, heating the growth table to 300 ℃, heating a gallium source to 1000 ℃, opening a baffle plate after the gallium source is stabilized, and introducing gallium atoms.
Monitoring growth gallium source flow rate by quartz crystal oscillator to be not higher than that of growth gallium source flow rateMonitoring gallium growth by Reflection High Energy Electron Diffraction (RHEED) and openingOxygen source is used for providing oxygen, radio frequency cracking is carried out on the oxygen, oxygen atoms (RF-O) after high frequency cracking are introduced, after the oxygen atoms are stabilized, a baffle is opened to enable the oxygen atoms to react with gallium atoms, and the reaction time is not less than 30 minutes.
Since the original amount of gallium atoms has been limited, the minimum time for oxygen to pass through the reaction is ensured. The flow rate of oxygen is controlled at 2.5sccm, the oxygen enrichment in the growth process is maintained, the power of radio frequency pyrolysis is set to be 250W, and the original Ga-O is destroyed by the excessive radio frequency pyrolysis power, so that the crystallinity of the product is not improved. And after oxygen atoms are introduced, the temperature of the growth table is increased to 550 ℃, so that the crystallinity of the beta-gallium oxide is improved.
After the growth is completed, the supply of the gallium source and oxygen source is stopped.
4. And cooling the grown two-dimensional beta-gallium oxide crystal film at a cooling rate of 1-30K/min. The stress can be reduced by controlling the cooling rate, which in this example is 20K/min.
5. The grown two-dimensional beta-gallium oxide crystal film is peeled from the beta-gallium oxide single crystal substrate, and the peeling can be performed by a mechanical peeling process, an ultrasonic peeling process or the like, and the details are not repeated here.
Referring to fig. 2, which shows an SEM (scanning electron microscope) image of a two-dimensional β -gallium oxide crystal thin film, fig. 3, which shows an AFM (atomic force microscope) image of a two-dimensional β -gallium oxide crystal thin film, it is known that the thin film thickness is about 1.6nm.
Fig. 4 is an SEM image and an AES (atomic emission spectroscopy) image of a two-dimensional β -gallium oxide crystal thin film, wherein (a) in fig. 4 is an SEM image, and (b), (C), and (d) are AES Mapping analysis images of O, ga and C, respectively. The grown film is a two-dimensional beta-gallium oxide crystal film, and the transverse dimension is 10-500 mu m.
The technical scheme shows that the application has the following beneficial effects:
according to the application, the homogeneous substrate is covered with the van der Waals material layer, and the high-quality two-dimensional beta-gallium oxide crystal film can be epitaxially grown on the van der Waals material layer by adopting a molecular beam epitaxy process, so that the method can be widely applied to power electronic devices, intelligent wearing and high-density batteries.
The detailed description set forth above in connection with the appended drawings describes exemplary embodiments, but does not represent all embodiments that may be implemented or fall within the scope of the claims. The term "exemplary" used throughout this specification means "serving as an example, instance, or illustration," and does not mean "preferred" or "advantageous over other embodiments. The detailed description includes specific details for the purpose of providing an understanding of the described technology. However, the techniques may be practiced without these specific details. In some instances, well-known structures and devices are shown in block diagram form in order to avoid obscuring the concepts of the described embodiments.
The previous description of the disclosure is provided to enable any person skilled in the art to make or use the disclosure. Various modifications to the disclosure will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other variations without departing from the scope of the disclosure. Thus, the disclosure is not limited to the examples and designs described herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for preparing a two-dimensional beta-gallium oxide crystal film, which is characterized by comprising the following steps:
s1, providing a beta-gallium oxide single crystal substrate;
s2, covering a van der Waals material layer on the beta-gallium oxide single crystal substrate;
and S3, epitaxially growing a two-dimensional beta-gallium oxide crystal film on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer by adopting a molecular beam epitaxy process.
2. The method for preparing a two-dimensional beta-gallium oxide crystal film according to claim 1, wherein the van der waals material layer is a graphene layer or a hexagonal boron nitride layer, and the thickness is 1-3 atomic layers.
3. The method for producing a two-dimensional β -gallium oxide crystal film according to claim 1, wherein the thickness of the van der waals material layer is 0.2nm to 2nm.
4. The method for preparing a two-dimensional β -gallium oxide crystal film according to claim 1, wherein the step S3 comprises:
providing a molecular beam epitaxy system having a gallium source and an oxygen source;
placing the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer on a growth table in a molecular beam epitaxy system, heating a gallium source to provide gallium atoms, closing an oxygen source, and growing a gallium layer on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer;
and opening an oxygen source to provide oxygen, performing radio frequency pyrolysis on the oxygen, and reacting oxygen atoms after the radio frequency pyrolysis with gallium atoms in an oxygen-enriched atmosphere to grow to obtain the two-dimensional beta-gallium oxide crystal film.
5. The method for preparing a two-dimensional beta-gallium oxide crystal film according to claim 4, wherein the heating temperature of the gallium source is 800 ℃ to 1100 ℃, and the flow rate of the gallium source isAnd/or the number of the groups of groups,
the oxygen flow provided by the oxygen source is 0.5 sccm-5 sccm; and/or the number of the groups of groups,
the power of the oxygen radio frequency pyrolysis is 200W-350W; and/or the number of the groups of groups,
the reaction time of the oxygen atoms and the gallium atoms is 30 min-300 min.
6. The method for preparing a two-dimensional beta-gallium oxide crystal film according to claim 4, wherein the molecular beam epitaxy process is carried out under vacuum condition at a pressure of 10 -7 Torr～10 -10 Torr。
7. The method for preparing a two-dimensional beta-gallium oxide crystal film according to claim 4, wherein the temperature of a growth stage in a molecular beam epitaxy system is 250 ℃ to 350 ℃ before the oxygen source is turned on; after the oxygen source is turned on, the temperature of a growth table in the molecular beam epitaxy system is 500-600 ℃.
8. The method for preparing a two-dimensional β -gallium oxide crystal film according to claim 1, wherein after step S2, further comprising:
and (3) carrying out an annealing process on the beta-gallium oxide single crystal substrate covered with the Van der Waals material layer under the vacuum condition, wherein the annealing temperature is 200-400 ℃, and the annealing time is 3-24 h.
9. The method for preparing a two-dimensional β -gallium oxide crystal film according to claim 1, wherein after step S3, further comprising:
and cooling the grown two-dimensional beta-gallium oxide crystal film at a cooling rate of 1-30K/min.
10. The method for preparing a two-dimensional β -gallium oxide crystal film according to claim 1, wherein after step S3, further comprising:
and stripping the grown two-dimensional beta-gallium oxide crystal film from the beta-gallium oxide single crystal substrate through a mechanical stripping process or an ultrasonic stripping process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311045476.2A CN116988148A (en) | 2023-08-18 | 2023-08-18 | Preparation method of two-dimensional beta-gallium oxide crystal film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311045476.2A CN116988148A (en) | 2023-08-18 | 2023-08-18 | Preparation method of two-dimensional beta-gallium oxide crystal film |
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