CN113643960B - beta-Ga based on pulse method 2 O 3 Film and method for producing the same - Google Patents
beta-Ga based on pulse method 2 O 3 Film and method for producing the same Download PDFInfo
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- CN113643960B CN113643960B CN202110632336.XA CN202110632336A CN113643960B CN 113643960 B CN113643960 B CN 113643960B CN 202110632336 A CN202110632336 A CN 202110632336A CN 113643960 B CN113643960 B CN 113643960B
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- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title description 2
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims abstract description 131
- 239000000758 substrate Substances 0.000 claims abstract description 68
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 34
- 229910052760 oxygen Inorganic materials 0.000 claims description 34
- 239000001301 oxygen Substances 0.000 claims description 34
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 claims description 30
- 238000000137 annealing Methods 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims 1
- 239000010408 film Substances 0.000 description 46
- 125000004429 atom Chemical group 0.000 description 20
- 239000010409 thin film Substances 0.000 description 11
- 238000013508 migration Methods 0.000 description 9
- 230000005012 migration Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 125000004430 oxygen atom Chemical group O* 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 4
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 4
- 229910001195 gallium oxide Inorganic materials 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02483—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02516—Crystal orientation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02609—Crystal orientation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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Abstract
The invention discloses a beta-Ga based on a pulse method 2 O 3 Film and preparation method thereof, beta-Ga 2 O 3 The film comprises: a homogeneous substrate layer, at least one pulse beta-Ga 2 O 3 Layer and at least one beta-Ga 2 O 3 A layer; the pulse beta-Ga 2 O 3 Number of layers and the beta-Ga 2 O 3 The number of layers is the same; the homogenous substrate layer and the beta-Ga 2 O 3 Between layers is grown with pulse beta-Ga 2 O 3 A layer; every two of the beta-Ga 2 O 3 Between layers is grown with pulse beta-Ga 2 O 3 A layer. The invention can epitaxially grow high-quality and low dislocation density beta-Ga on the basis of a pulse method 2 O 3 A film.
Description
Technical Field
The invention belongs to the field of semiconductor materials, and in particular relates to a beta-Ga based on a pulse method 2 O 3 A film and a method for preparing the same.
Background
β-Ga 2 O 3 The film has great application potential in high-power high-breakdown devices, so with the wide application of the high-power high-breakdown devices, the film has great application potential to beta-Ga 2 O 3 The requirements for films are also increasing.
In the prior art, beta-Ga is generally carried out on the basis of a homogeneous substrate layer 2 O 3 Preparation of film for preparation of beta-Ga 2 O 3 The values of all growth parameters of the film must be reasonably adjusted, so that the preparation method in the prior art is complex, and the quality is difficult to ensure. In addition, when the quality of the homogenous substrate layer is poor, it is nowThe prior art fails to perform beta-Ga based on the poor quality homogenous substrate layer 2 O 3 And (3) preparing a film.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a beta-Ga based on a pulse method 2 O 3 A film and a method for preparing the same. The technical problems to be solved by the invention are realized by the following technical scheme:
beta-Ga based on pulse method 2 O 3 Film of beta-Ga 2 O 3 The film comprises: a homogeneous substrate layer, at least one pulse beta-Ga 2 O 3 Layer and at least one beta-Ga 2 O 3 A layer; the pulse beta-Ga 2 O 3 Number of layers and the beta-Ga 2 O 3 The number of layers is the same; the homogenous substrate layer and the beta-Ga 2 O 3 Between layers is grown with pulse beta-Ga 2 O 3 A layer; every two of the beta-Ga 2 O 3 Between layers is grown with pulse beta-Ga 2 O 3 A layer.
In one embodiment of the invention, the pulse is beta-Ga 2 O 3 The thickness of the layer is 30-50nm.
In one embodiment of the invention, the pulse is beta-Ga 2 O 3 The layer is of monocrystalline structure.
The invention has the beneficial effects that:
the invention can epitaxially grow high-quality and low dislocation density beta-Ga on the basis of a pulse method 2 O 3 A film.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 shows a pulse-based beta-Ga 2 O 3 A film structure schematic diagram;
FIG. 2 shows a pulse-based beta-Ga 2 O 3 A flow diagram of a film preparation method;
FIG. 3 is a timing flow chart of a pulse method according to an embodiment of the present invention;
FIG. 4 shows a pulse-based beta-Ga 2 O 3 Schematic diagram of film preparation process.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but embodiments of the present invention are not limited thereto.
Example 1
Referring to FIG. 1, FIG. 1 shows a pulse-based beta-Ga method according to an embodiment of the present invention 2 O 3 Schematic of film structure, beta-Ga 2 O 3 The film comprises: a homogeneous substrate layer, at least one pulse beta-Ga 2 O 3 Layer and at least one beta-Ga 2 O 3 A layer.
The invention is based on the substrate layer for epitaxial layer growth to obtain a thin film material, and when the epitaxial layer and the substrate layer are of the same material, the substrate layer is called a homogeneous substrate layer. The invention aims to prepare beta-Ga 2 O 3 A (gallium oxide) film, said homogeneous substrate layer also known as Ga 2 O 3 A (gallium oxide) substrate layer.
Optionally, the pulse is beta-Ga 2 O 3 Number of layers and the beta-Ga 2 O 3 The number of layers is the same.
Optionally, the homogenous substrate layer and the beta-Ga 2 O 3 Between layers is grown with pulse beta-Ga 2 O 3 A layer.
Alternatively, every two of said beta-Ga 2 O 3 Between layers is grown with pulse beta-Ga 2 O 3 A layer.
beta-Ga is generally prepared 2 O 3 In the case of thin films, the substrate layer is homogeneous with beta-Ga 2 O 3 Between layers, beta-Ga 2 O 3 Layer and beta-Ga 2 O 3 Between layers, the prepared beta-Ga can be caused due to the problems of lattice mismatch, thermal mismatch and the like 2 O 3 The thin film contains a large number of defects such as dislocations, and in general, the dislocation extends in a direction along with the increase in the thickness of the thin filmSimilarly, the defect reduces beta-Ga 2 O 3 The quality of the film. In particular, a thin film is prepared while maintaining a fixed growth mode, and as the thickness of the prepared thin film increases, dislocations in the thin film gradually extend, even from the surface of the substrate to the surface of the epitaxial layer, severely affecting the quality of the prepared thin film.
The invention is characterized in that beta-Ga 2 O 3 Introduction of pulsed beta-Ga into films 2 O 3 A layer of pulsed beta-Ga 2 O 3 The layer is used as buffer layer to effectively prevent dislocation from extending in the film, thereby reducing dislocation density in the film and improving the beta-Ga 2 O 3 Film quality. Specifically, a layer of pulse beta-Ga is firstly introduced into a homogeneous substrate layer 2 O 3 A layer of pulsed beta-Ga 2 O 3 The layer can reduce the homogeneous substrate layer and beta-Ga 2 O 3 Lattice mismatch between layers, thereby reducing dislocation density; second, growing beta-Ga 2 O 3 In the course of the layers, in every two layers of beta-Ga 2 O 3 Introduction of pulsed beta-Ga between layers 2 O 3 Layer, growing the beta-Ga 2 O 3 The layer is a growth module for growing the pulse beta-Ga 2 O 3 The layer is in another growth mode, and the growth beta-Ga can be repaired by changing the growth mode 2 O 3 Dislocation extending longitudinally in the layer, thereby reducing every two beta-Ga 2 O 3 Dislocation density between layers.
In addition, in the prior art, two paths of reaction source gases of a Ga source and an O source are simultaneously introduced into a reaction chamber, so that the bonding speed of Ga atoms and O atoms is very high, and atoms are bonded with each other when the atoms are not migrated to an ideal position on the surface, therefore, the migration length of the atoms is low, three-dimensional nucleation growth is caused, and the surface is rough. The invention grows the pulse beta-Ga by a pulse method 2 O 3 In the layer, two paths of gases of Ga source and O source are wrongly introduced into the reaction chamber according to respective pulse time parameters, so that the migration time of reaction atoms on the surface is increased, the transverse migration length of atoms on the surface is effectively increased, the two-dimensional nucleation growth is enhanced, the atoms are combined to the most suitable position,improves the surface flatness and can further improve the prepared beta-Ga 2 O 3 Film quality.
The pulse beta-Ga 2 O 3 Layer and beta-Ga 2 O 3 The number of layers is set by those skilled in the art according to the service requirement, and the present invention is not limited. Referring to FIG. 1, three pulses of beta-Ga are used in FIG. 1 2 O 3 Layers and three beta-Ga 2 O 3 The layers are illustrated as a homogeneous substrate layer 1, pulse beta-Ga, in order from bottom to top 2 O 3 Layer 2, beta-Ga 2 O 3 Layer 3, pulse beta-Ga 2 O 3 Layer 4, beta-Ga 2 O 3 Layer 5, pulse beta-Ga 2 O 3 Layer 6, pulse beta-Ga 2 O 3 Layer 7.
Wherein the pulse is beta-Ga 2 O 3 Layer 2 is capable of preventing homogeneous substrate layer 1 from being mixed with beta-Ga 2 O 3 Dislocation extension between layers 3, further, pulse beta-Ga 2 O 3 Layer 4 is capable of blocking beta-Ga 2 O 3 Layer 3 and beta-Ga 2 O 3 Dislocation propagation between layers 5, further, pulsed beta-Ga 2 O 3 Layer 6 is capable of blocking beta-Ga 2 O 3 Layer 5 and beta-Ga 2 O 3 Dislocation propagation between layers 7, the present invention is achieved by multilayer pulsing beta-Ga 2 O 3 Layers capable of more effectively consolidating and improving beta-Ga 2 O 3 Flatness of the film.
Optionally, the pulse is beta-Ga 2 O 3 The thickness of the layer is 30-50nm.
The pulsed beta-Ga is verified by experiments by a person skilled in the art 2 O 3 The thickness of the layer is set to 30-50nm, which can ensure the preparation of beta-Ga 2 O 3 While improving the film quality, the pulse beta-Ga 2 O 3 The growth rate of the layer, thereby increasing beta-Ga 2 O 3 The preparation efficiency of the film.
Optionally, the pulse is beta-Ga 2 O 3 The layer is of monocrystalline structure.
Through experimental verification by those skilled in the art, phaseWhen the pulse is beta-Ga compared with a polycrystalline structure or an amorphous structure 2 O 3 When the layer is of a single crystal structure, the beta-Ga is prepared 2 O 3 The thin film has better electrical properties, smaller dislocation density and lower roughness.
In conclusion, the invention can obtain the pulse beta-Ga by a pulse method 2 O 3 A layer based on the pulse beta-Ga 2 O 3 The beta-Ga 2O3 film with high quality and low dislocation density is epitaxially grown outside the homogeneous substrate layer.
Example two
Referring to FIG. 2, FIG. 2 is a diagram showing a pulse-based beta-Ga method according to an embodiment of the present invention 2 O 3 The flow chart of the film preparation method is shown in the schematic diagram. The method comprises the following steps:
step 1: performing thermal annealing treatment on the homogeneous substrate layer according to preset thermal annealing parameters to obtain a target substrate layer, wherein the preset thermal annealing parameters comprise: a first reactor temperature parameter, a first oxygen flow parameter, a nitrogen flow parameter, and a thermal annealing time parameter.
Optionally, the step 1 includes:
step 1-1: and placing the homogeneous substrate layer into a preset reaction chamber.
Step 1-2: and carrying out thermal annealing treatment on the pair of homogeneous substrate layers in a preset reaction chamber according to preset thermal annealing parameters.
The invention is based on the substrate layer for epitaxial layer growth to obtain a thin film material, and when the epitaxial layer and the substrate layer are of the same material, the substrate layer is called a homogeneous substrate layer. The invention aims to prepare beta-Ga 2 O 3 A (gallium oxide) film, said homogeneous substrate layer also known as Ga 2 O 3 A (gallium oxide) substrate layer.
When the epitaxial growth of the thin film is performed based on the substrate layer, it is necessary to perform a thermal annealing treatment for flattening the surface of the substrate layer and passivating dangling bonds on the surface of the substrate layer to obtain a target substrate layer on which the high-quality epitaxial layer can be grown, thereby obtaining a high-quality thin film.
The invention carries out thermal annealing treatment of the homogeneous substrate layer and pulse beta-Ga through the preset reaction chamber 2 O 3 Layer growth and beta-Ga 2 O 3 Layer growth to produce beta-Ga 2 O 3 The film, the preset reaction chamber is selected by a person skilled in the art according to the service requirement, and the invention is not particularly limited. In the present invention, the preset chamber is exemplified by a low pressure MOCVD (Metal-Organic Chemical Vapor Deposition, metalorganic chemical vapor deposition) chamber.
The preset annealing parameters are set in the preset reaction chamber according to the service requirement by a person skilled in the art, and the invention is not limited. Experiments prove that the preset thermal annealing parameters are preferably set as follows: the first chamber temperature parameter is 900 ℃, the first oxygen flow parameter is 2100sccm, the nitrogen flow parameter is 1000sccm, and the thermal annealing time parameter is 15min.
Step 2: according to the first growth parameter, carrying out pulse treatment on the target substrate layer to grow on the surface of the target substrate layer to obtain pulse beta-Ga 2 O 3 A layer.
Optionally, the first growth parameter includes: first triethyl gallium flow parameter, second oxygen flow parameter, triethyl gallium TEGa pulse time parameter and oxygen O 2 Pulse time parameters and pulse period parameters.
The preset reaction chamber is provided with a first growth parameter, and the first growth parameter is set by a person skilled in the art according to service requirements, so that the invention is not limited. Experiments prove that the preset thermal annealing parameters are preferably set as follows: the first growth parameters include: a first triethylgallium flow parameter 40sccm, a second oxygen flow parameter 2100sccm, a triethylgallium pulse time parameter 0.1min, an oxygen pulse time parameter 0.3min, and a pulse period parameter: 30 cycles (or 12 min).
Optionally, the first growth parameter further includes: second reaction chamber temperature, growth pressure parameters.
Experiments prove that the preset thermal annealing parameters are preferably set as follows: the second reaction chamber temperature was 800℃and the growth pressure parameter was 40Torr.
Optionally, the step 2 includes:
step 2-1: and introducing triethyl gallium into the preset reaction chamber according to the first triethyl gallium flow parameter and the triethyl gallium pulse time parameter.
Step 2-2: and introducing oxygen into the preset reaction chamber according to the second oxygen flow parameter and the parameter oxygen pulse time parameter.
In a pulse period divided into a triethylgallium pulse time and an oxygen pulse time, for example, a triethylgallium pulse time parameter of 0.1min and an oxygen pulse time parameter of 0.3min, one pulse period is 0.4min, i.e., the steps 2-1 and 2-2 are performed in one pulse period.
Referring to fig. 3, a timing flow chart of a pulse method according to an embodiment of the present invention is shown, in fig. 3, a vertical axis indicates a reaction source switch (preforfluoride), on indicates on, off indicates off, a vertical axis indicates a pulse Time (Time), a waveform bump indicates on, and a recess indicates off.
Specifically, when the triethyl gallium waveform is concave and the oxygen waveform is convex within 0.0-0.3min, the preset reaction chamber starts to be filled with oxygen, and simultaneously, the supply of the triethyl gallium is stopped; and when the triethyl gallium waveform is convex and the oxygen waveform is concave within 0.3-0.4min, starting to introduce the triethyl gallium into the preset reaction chamber, and stopping introducing the oxygen.
The pulse method is characterized in that when a preset reaction chamber is filled with triethyl gallium according to a first triethyl gallium flow parameter and the triethyl gallium pulse time parameter, the preset reaction chamber stops filling oxygen; or when the preset reaction chamber is filled with oxygen according to the second oxygen flow parameter and the parameter oxygen pulse time parameter, stopping filling the triethyl gallium into the preset reaction chamber.
In the prior art, two paths of reaction source gases of a Ga source and an O source are simultaneously introduced into a reaction chamber, so that the bonding speed of Ga atoms and O atoms is very high, atoms are bonded with each other when the atoms are not migrated to ideal positions on the surface, and therefore, the migration length of the atoms is low, and three-dimensional nucleation growth can be caused. Further, since the mobility of Ga atoms is different from that of O atoms, ga atoms are smaller than that of O atoms as metal atoms, and therefore the migration length of Ga atoms is smaller than that of O atoms at the same time, when the reaction source gas is simultaneously introduced, surface roughness is caused.
The invention grows the pulse beta-Ga by a pulse method 2 O 3 When in layer, two paths of gases of Ga source and O source are staggered and introduced into the reaction chamber according to respective pulse time parameters, and the migration time of the atoms of various reaction sources on the surface can be reasonably set by adjusting the time of each path of pulse according to different migration lengths of various reaction atoms, so that the transverse migration length of the atoms on the surface is enhanced, the atoms are combined to the most suitable position, and finally, the two-dimensional growth of the film is realized, thereby improving the quality of the film. For example, 0.1minO+0.3minGa, i.e., a longer pulse time is given to the Ga source, and the migration length of Ga atoms is increased, so that the two-dimensional growth of the film can be effectively improved.
Step 2-3: repeating the step 2-1 and the step 2-2 according to the pulse period parameters to grow on the surface of the thermally annealed homogeneous substrate layer to obtain the pulse beta-Ga 2 O 3 A layer.
The pulse period parameter refers to the number of times the steps 2-1 and 2-2 are repeated, for example, the pulse period parameter is 30 periods, i.e., steps 2-1 and 2-2 are repeatedly performed 30 times to obtain 30 periods of beta-Ga 2 O 3 A layer.
Step 3: according to a second growth parameter, in said pulse beta-Ga 2 O 3 Growing the surface of the layer to obtain beta-Ga 2 O 3 A layer.
Optionally, the second growth parameters include: a second triethylgallium flow parameter, a third oxygen flow parameter, and a growth time parameter.
The preset reaction chamber is provided with a second growth parameter, and the second growth parameter is set by a person skilled in the art according to service requirements, so that the invention is not limited. The second triethylgallium flow parameter and the third oxygen flow parameter in the second growth parameter may be the same value as the first triethylgallium flow parameter and the second oxygen flow parameter in the first growth parameter. Experiments prove that the preset thermal annealing parameters are preferably set as follows: the second triethyl gallium flow parameter is 40sccm, the third oxygen flow parameter is 2100sccm, and the growth time parameter is 20min.
Optionally, said pulse is beta-Ga according to a second growth parameter 2 O 3 Growing the surface of the layer to obtain beta-Ga 2 O 3 A layer, comprising:
simultaneously introducing triethyl gallium and oxygen into the preset reaction chamber according to the second triethyl gallium flow parameter, the third oxygen flow parameter and the growth time parameter so as to obtain the pulse beta-Ga 2 O 3 Growing the surface of the layer to obtain beta-Ga 2 O 3 A layer.
Optionally, after the step 3, the method further includes:
step S11: subjecting the beta-Ga to 2 O 3 The layer serves as a new target substrate layer.
Step S12: repeating the step 2 and the step 3 according to preset preparation parameters to obtain the target beta-Ga 2 O 3 A film.
The invention can grow the beta-Ga 2 O 3 The layer is used as a new target substrate layer for preparing the substrate layer with at least one pulse beta-Ga 2 O 3 Layer and at least one beta-Ga 2 O 3 beta-Ga of a layer 2 O 3 Films, generally referred to as beta-Ga 2 O 3 The film has at least two pulses of beta-Ga 2 O 3 Layer and at least two beta-Ga 2 O 3 A layer.
Referring to fig. 1, a pulse-based beta-Ga method is provided in an embodiment of the present invention 2 O 3 Film structure schematic, three pulse beta-Ga is used in figure 1 2 O 3 Layers and three beta-Ga 2 O 3 The layers are illustrated. Wherein the pulse is beta-Ga 2 O 3 Layer 2 can preventHomogeneous substrate layer 1 and beta-Ga 2 O 3 Dislocation extension between layers 3, further, pulse beta-Ga 2 O 3 Layer 4 is capable of blocking beta-Ga 2 O 3 Layer 3 and beta-Ga 2 O 3 Dislocation propagation between layers 5, further, pulsed beta-Ga 2 O 3 Layer 6 is capable of blocking beta-Ga 2 O 3 Layer 5 and beta-Ga 2 O 3 Dislocation propagation between layers 7, the present invention is achieved by multilayer pulsing beta-Ga 2 O 3 Layers capable of more effectively consolidating and improving beta-Ga 2 O 3 Flatness of the film.
The invention is characterized in that beta-Ga 2 O 3 Introduction of pulsed beta-Ga into films 2 O 3 A layer of pulsed beta-Ga 2 O 3 The layer is used as buffer layer to effectively prevent dislocation from extending in the film, thereby reducing dislocation density in the film and improving the beta-Ga 2 O 3 Film quality. In addition, the pulse beta-Ga 2 O 3 The layer has the characteristics of high flatness and the like, and can further improve the prepared beta-Ga 2 O 3 Film quality.
Optionally, before the step 1, the method further includes:
step S21: and polishing the homogeneous substrate layer.
Step S22: and placing the polished homogeneous substrate layer into a prefabricated solution for soaking treatment.
The soaking treatment can enable pollutants on the surface of the homogeneous substrate layer to fall off more easily. For example, the pre-formed solution is a 30% HF acid solution and the homogenous substrate layer is immersed in the 30% HF acid solution for 60s.
Step S23: and cleaning the soaked homogeneous substrate layer.
The cleaning process is capable of removing contaminants, such as organic and inorganic contaminants, from the surface of the homogenous substrate layer. For example, the contaminants on the surface of the homogenous substrate layer are removed with alcohol and acetone.
Step S24: and washing the cleaned homogeneous substrate layer.
The rinsing process is capable of rinsing away the chemical solution from the surface of the homogeneous substrate. For example, rinse with flowing deionized water for 60s.
Referring to FIG. 4, a pulse-based beta-Ga is provided in an embodiment of the present invention 2 O 3 Schematic diagram of film preparation process.
In conclusion, the invention can obtain the pulse beta-Ga by a pulse method 2 O 3 A layer based on the pulse beta-Ga 2 O 3 The beta-Ga 2O3 film with high quality and low dislocation density is epitaxially grown outside the homogeneous substrate layer.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present invention, unless expressly stated or limited otherwise, a first feature "above" or "below" a second feature may include both the first and second features being in direct contact, as well as the first and second features not being in direct contact but being in contact with each other through additional features therebetween. Moreover, a first feature being "above," "over" and "on" a second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature includes the first feature being directly under and obliquely below the second feature, or simply means that the first feature is less level than the second feature.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Further, one skilled in the art can engage and combine the different embodiments or examples described in this specification.
Although the present application has been described herein in connection with various embodiments, other variations to the disclosed embodiments can be understood and effected by those skilled in the art in practicing the claimed application, from a review of the figures, the disclosure, and the appended claims. In the claims, the word "comprising" does not exclude other elements or steps, and the "a" or "an" does not exclude a plurality. A single processor or other unit may fulfill the functions of several items recited in the claims. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used to advantage.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (9)
1. beta-Ga based on pulse method 2 O 3 A film characterized in that the beta-Ga 2 O 3 The film comprises: homogeneous substrate layer, multiple pulses of beta-Ga 2 O 3 Layers and a plurality of beta-Ga 2 O 3 A layer;
the pulse beta-Ga 2 O 3 Number of layers and the beta-Ga 2 O 3 The number of layers is the same;
the homogenous substrate layer and the beta-Ga 2 O 3 Between layers is grown with pulse beta-Ga 2 O 3 A layer;
every two of the beta-Ga 2 O 3 Between layers is grown with pulse beta-Ga 2 O 3 A layer.
2. beta-Ga according to claim 1 2 O 3 A film characterized in that the pulse beta-Ga 2 O 3 The thickness of the layer is 30-50nm.
3. beta-Ga according to claim 1 2 O 3 A film characterized in that the pulse beta-Ga 2 O 3 The layer is of monocrystalline structure.
4. beta-Ga based on pulse method 2 O 3 A method of producing a film, the method comprising:
step 1: performing thermal annealing treatment on the homogeneous substrate layer according to preset thermal annealing parameters to obtain a target substrate layer, wherein the preset thermal annealing parameters comprise: a first reactor temperature parameter, a first oxygen flow parameter, a nitrogen flow parameter, and a thermal annealing time parameter;
step 2: according to the first growth parameter, carrying out pulse treatment on the target substrate layer to grow on the surface of the target substrate layer to obtain pulse beta-Ga 2 O 3 A layer, wherein the first growth parameters include: first triethyl gallium flow parameter, second oxygen flow parameter and triethylA gallium based pulse time parameter, an oxygen pulse time parameter, and a pulse period parameter;
step 3: according to a second growth parameter, in said pulse beta-Ga 2 O 3 Growing the surface of the layer to obtain beta-Ga 2 O 3 A layer, wherein the second growth parameters comprise: a second triethylgallium flow parameter, a third oxygen flow parameter, and a growth time parameter.
5. The method according to claim 4, wherein the step 1 comprises:
step 1-1: placing the homogeneous substrate layer into a preset reaction chamber;
step 1-2: and carrying out thermal annealing treatment on the pair of homogeneous substrate layers in a preset reaction chamber according to preset thermal annealing parameters.
6. The method according to claim 5, wherein step 2 comprises:
step 2-1: introducing triethyl gallium into the preset reaction chamber according to the first triethyl gallium flow parameter and the triethyl gallium pulse time parameter;
step 2-2: introducing oxygen into the preset reaction chamber according to the second oxygen flow parameter and the oxygen pulse time parameter;
step 2-3: repeating the step 2-1 and the step 2-2 according to the pulse period parameters to grow on the surface of the thermally annealed homogeneous substrate layer to obtain the pulse beta-Ga 2 O 3 A layer.
7. The method of claim 5, wherein said pulse is beta-Ga according to a second growth parameter 2 O 3 Growing the surface of the layer to obtain beta-Ga 2 O 3 A layer, comprising:
simultaneously introducing triethyl gallium and oxygen into the preset reaction chamber according to the second triethyl gallium flow parameter, the third oxygen flow parameter and the growth time parameter so as to obtain the pulse beta-Ga 2 O 3 Growing the surface of the layer to obtain beta-Ga 2 O 3 A layer.
8. The method according to claim 4, wherein after step 3, the method further comprises:
subjecting the beta-Ga to 2 O 3 The layer serves as a new target substrate layer;
repeating the step 2 and the step 3 according to preset preparation parameters to obtain the target beta-Ga 2 O 3 A film.
9. The method according to claim 4, wherein prior to step 1, the method further comprises:
polishing the homogeneous substrate layer;
placing the polished homogeneous substrate layer into a prefabricated solution for soaking treatment;
cleaning the soaked homogeneous substrate layer;
and washing the cleaned homogeneous substrate layer.
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