CN113571404B - Beta-Ga2O3Method for growing thin film - Google Patents
Beta-Ga2O3Method for growing thin film Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims description 14
- 239000000758 substrate Substances 0.000 claims abstract description 50
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 46
- 239000010980 sapphire Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 37
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 239000010408 film Substances 0.000 claims description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims 4
- 230000007704 transition Effects 0.000 abstract description 8
- 230000003746 surface roughness Effects 0.000 abstract description 3
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 32
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 19
- 239000000463 material Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000006467 substitution reaction Methods 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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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
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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
- H01L21/02436—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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- 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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- 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 relates to a growth method of a beta-Ga 2O3 film, which comprises the following steps: selecting a sapphire substrate; growing (Al x1Ga1‑x1)2O3 buffer layer under T 1 temperature conditions, growing (Al x2Ga1‑x2)2O3 buffer layer under T 2 temperature conditions) on the sapphire substrate (Al x1Ga1‑x1)2O3 buffer layer; growing (Al x3Ga1‑x3)2O3 buffer layer, x1 > x2 > x3; A β -Ga 2O3 film, T 1＜T2＜T3＜T4, was grown on (Al x3Ga1‑x3)2O3 buffer layer) at a temperature of T 4. The invention introduces a variable-temperature growth (Al 1‑xGax)2O3 buffer layer between the beta-Ga 2O3 film and the sapphire substrate, and the introduction of the (Al 1‑xGax)2O3 buffer layer) not only realizes the uniform transition of element components between the substrate and the film, but also realizes the transition of lattice structures, thereby reducing lattice mismatch induced dislocations. According to the difference of element components among buffer layers, different growth temperatures are adopted, so that the growth quality of the buffer layers is improved, the two-dimensional growth of the beta-Ga 2O3 film is enhanced, and the surface roughness of the film is reduced.
Description
Technical Field
The invention belongs to the technical field of semiconductor film growth, and relates to a method for growing a beta-Ga 2O3 film.
Background
With the increasing performance requirements of semiconductor devices, conventional Si-based devices are increasingly challenged with lower breakdown voltages that are increasingly difficult to apply in the field of high breakdown high power devices. beta-Ga 2O3 as a third generation semiconductor material has a forbidden band width of up to 5eV, which makes its breakdown voltage and breakdown electric field far greater than Si material, and its Barlish figure of merit far greater than GaN etc. third generation semiconductor material, so beta-Ga 2O3 has great potential in application in electronic devices.
Ga 2O3 semiconductor materials have 5 different structures, alpha-, beta-, gamma-, delta-, epsilon-, respectively. Among the most stable and most applicable are beta-Ga 2O3. Heteroepitaxy with respect to the β -Ga 2O3 film is mainly focused on the sapphire substrate, however, the epitaxial β -Ga 2O3 film has more dislocations and higher surface roughness, which makes it difficult to apply in electronic devices.
New epitaxial methods must therefore be employed to reduce the dislocation and surface roughness of beta-Ga 2O3 and thereby improve the crystalline quality of beta-Ga 2O3.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for growing a beta-Ga 2O3 film. The technical problems to be solved by the invention are realized by the following technical scheme:
The embodiment of the invention provides a growth method of a beta-Ga 2O3 film, which comprises the following steps:
Selecting a sapphire substrate;
Growing (Al x1Ga1-x1)2O3 buffer layer;
Growing (Al x2Ga1-x2)2O3 buffer layer on the (Al x1Ga1-x1)2O3 buffer layer;
Growing (Al x3Ga1-x3)2O3 buffer layer, wherein x1 > x2 > x3, on the (Al x2Ga1-x2)2O3 buffer layer at a temperature of T 3;
A β -Ga 2O3 film was grown on the (Al x3Ga1-x3)2O3 buffer layer) at a temperature of T 4 a, wherein T 1＜T2＜T3＜T4.
In one embodiment of the invention, the sapphire substrate comprises a c-plane sapphire substrate.
In one embodiment of the present invention, selecting a sapphire substrate includes:
and placing the sapphire substrate into an HF acid solution for soaking, then washing the soaked sapphire substrate by using alcohol and acetone, then washing the washed sapphire substrate by using flowing deionized water, and finally drying the washed sapphire substrate by using high-purity nitrogen.
In one embodiment of the invention, the T 1 is 450-550 ℃, the T 2 is 550-650 ℃, the T 3 is 650-750 ℃, and the T 4 is 750-850 ℃.
In one embodiment of the present invention, an Al x1Ga1-x1)2O3 buffer layer is grown on the sapphire substrate under the temperature condition of T 1 (comprising:
And growing the (Al x1Ga1-x1)2O3 buffer layer) on the sapphire substrate by utilizing an MOCVD process at the temperature of 450-550 ℃, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled at 35-45Torr, the TEAL flow is 38-42sccm, the TEGa flow is 8-12sccm, and the growth time is 3-5min.
In one embodiment of the present invention, a layer of (Al x2Ga1-x2)2O3 buffer layer, including:
closing TEAL and TEGa, and raising the temperature to 550-650 ℃;
and opening TEAL and TEGa, and growing the (Al x2Ga1-x2)2O3 buffer layer on the (Al x1Ga1-x1)2O3 buffer layer) by using an MOCVD process at the temperature of 550-650 ℃, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled to be 35-45Torr, the TEAL flow is 22-28sccm, the TEGa flow is 22-28sccm, and the growth time is 3-5min.
In one embodiment of the present invention, a layer of (Al x3Ga1-x3)2O3 buffer layer, including:
Closing TEAL and TEGa, and increasing the temperature to 650-750 ℃;
And opening TEAL and TEGa, and growing the (Al x3Ga1-x3)2O3 buffer layer on the (Al x2Ga1-x2)2O3 buffer layer) by using an MOCVD process at the temperature of 650-750 ℃, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled to be 35-45Torr, the TEAL flow is 8-12sccm, the TEGa flow is 38-42sccm, and the growth time is 3-5min.
In one embodiment of the present invention, a beta-Ga 2O3 film is grown on the (Al x3Ga1-x3)2O3 buffer layer under the temperature condition of T 4, comprising
Closing TEAL and TEGa, heating to 900-950 ℃ for 25-35min, and then reducing the temperature to 750-850 ℃;
And (3) keeping TEAL closed, opening TEGa, and growing the beta-Ga 2O3 film on the (Al x3Ga1-x3)2O3 buffer layer) by using an MOCVD process at the temperature of 750-850 ℃, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled at 35-45Torr, the TEGa flow is 45-55sccm, and the growth time is 55-65min.
In one embodiment of the invention, x1 is 0.7-0.9, x2 is 0.4-0.6, and x3 is 0.1-0.3.
In one embodiment of the present invention, the thickness of the (Al x1Ga1-x1)2O3 buffer layer, the (Al x2Ga1-x2)2O3 buffer layer, and the (Al x3Ga1-x3)2O3 buffer layer) ranges from 30 to 50nm.
Compared with the prior art, the invention has the beneficial effects that:
According to the invention, a variable-temperature growth (Al 1-xGax)2O3 buffer layer) is introduced between the beta-Ga 2O3 film and the sapphire substrate in the traditional growth process, and because of different lattice structures between the beta-Ga 2O3 film and the sapphire substrate, the introduction of the Al 1-xGax)2O3 buffer layer not only realizes uniform transition of element components between the substrates, but also realizes transition of the lattice structures, thereby reducing dislocation caused by lattice mismatch.
Other aspects and features of the present invention will become apparent from the following detailed description, which refers to the accompanying drawings. It is to be understood that the drawings are designed solely for purposes of illustration and not as a definition of the limits of the invention, for which reference should be made to the appended claims. It should be further understood that the drawings are not necessarily drawn to scale and that, unless otherwise indicated, they are merely intended to conceptually illustrate the structures and procedures described herein.
Drawings
FIG. 1 is a schematic flow chart of a method for growing a beta-Ga 2O3 film according to an embodiment of the present invention;
Fig. 2 is a schematic diagram of a preparation process of a method for growing a β -Ga 2O3 thin film according to an embodiment of the present invention.
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 and fig. 2, fig. 1 is a schematic flow chart of a method for growing a β -Ga 2O3 thin film according to an embodiment of the present invention, and fig. 2 is a schematic preparation process diagram of a method for growing a β -Ga 2O3 thin film according to an embodiment of the present invention. The invention provides a growth method of a beta-Ga 2O3 film, which comprises the following steps:
and 1, selecting a sapphire substrate 1.
Specifically, the sapphire substrate is placed into an HF acid solution for soaking, then the soaked sapphire substrate is cleaned by alcohol and acetone, then the cleaned sapphire substrate is rinsed by flowing deionized water, and finally the rinsed sapphire substrate is dried by high-purity nitrogen.
Preferably, the HF acid solution consists of a solution with an HF acid content of 30%.
Preferably, the sapphire substrate 1 comprises a chemically mechanically polished c-plane sapphire substrate.
And 2, growing (Al x1Ga1-x1)2O3 buffer layer 2) on the sapphire substrate 1 under the temperature condition of T 1.
Specifically, MOCVD (Metal-organic Chemical Vapor Deposition, metal organic chemical vapor deposition) process is utilized to grow (Al x1Ga1-x1)2O3 buffer layer 2, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled at 35-45Torr, the TEAL (triethylaluminum) flow is 38-42sccm, the TEGa (triethylgallium) flow is 8-12sccm, and the growth time is 3-5 min) on the sapphire substrate 1 at the temperature of 450-550 ℃.
For example, the cleaned sapphire substrate 1 was placed in a low-pressure MOCVD reactor, the flow rate of oxygen was set at 2100sccm, the flow rate of nitrogen was set at 1000sccm, the growth pressure was controlled at 40torr, the flow rates of teal and TEGa were 40 and 10sccm, respectively, the growth temperature was 500 ℃, and the growth was 3 to 5 minutes (Al x1Ga1-x1)2O3 buffer layer 2.
Preferably, T 1 is 450-550 ℃.
Preferably, x1 is 0.7-0.9.
Preferably, the thickness of the (Al x1Ga1-x1)2O3) buffer layer 2 is in the range of 30-50nm.
And 3, growing (Al x2Ga1-x2)2O3 buffer layer 3) on the (Al x1Ga1-x1)2O3 buffer layer 2 under the temperature condition of T 2.
Specifically, TEAL and TEGa are closed, and the temperature is raised to 550-650 ℃; and (3) opening TEAL and TEGa, and growing on the (Al x1Ga1-x1)2O3 buffer layer 2 by using an MOCVD process at the temperature of 550-650 ℃ (Al x2Ga1-x2)2O3 buffer layer 3, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled at 35-45Torr, the TEAL flow is 22-28sccm, the TEGa flow is 22-28sccm, and the growth time is 3-5min.
For example, based on step 2, firstly, the TEAl and TEGa flows are turned off, and other growth parameters are kept unchanged, the growth temperature is raised to 600 ℃, then, the TEAl and TEGa flows are turned on, the TEAl and TEGa flows are controlled to 25sccm and 25sccm respectively, and the growth is continued for 3-5min (Al x2Ga1-x2)2O3 buffer layer 3.
Preferably, T 2 is 550-650 ℃.
Preferably, x2 is 0.4-0.6.
Preferably, the thickness of the (Al x2Ga1-x2)2O3) buffer layer 3 is in the range of 30-50nm.
Step 4, growing (Al x3Ga1-x3)2O3 buffer layer 4, wherein x1 > x2 > x 3) on the (Al x2Ga1-x2)2O3 buffer layer 3 under the temperature condition of T 3.
Specifically, TEAL and TEGa are closed, and the temperature is increased to 650-750 ℃; and (3) opening TEAL and TEGa, and growing on the (Al x2Ga1-x2)2O3 buffer layer 3 by using an MOCVD process at the temperature of 650-750 ℃ (Al x3Ga1-x3)2O3 buffer layer 4, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled to be 35-45Torr, the TEAL flow is 8-12sccm, the TEGa flow is 38-42sccm, and the growth time is 3-5 min).
For example, on the basis of step 3, firstly, the TEAl and TEGa flows are turned off, and other growth parameters are kept unchanged, the growth temperature is raised to 700 ℃, then, the TEAl and TEGa flows are turned on, the TEAl and TEGa flows are controlled to 10 sccm and 40sccm respectively, and the (Al x3Ga1-x3)2O3 buffer layer 4 is grown again for 3-5 min.
Preferably, T 3 is 650-750deg.C.
Preferably, x3 is 0.1-0.3.
Preferably, the thickness of the (Al x3Ga1-x3)2O3) buffer layer 4 is in the range of 30-50nm.
And 5, growing a beta-Ga 2O3 film 5 on the (Al x3Ga1-x3)2O3 buffer layer 4 at the temperature of T 4, wherein T 1＜T2＜T3＜T4.
Specifically, TEAL and TEGa are closed, the temperature is raised to 900-950 ℃ and is thermally annealed for 25-35min, and then the temperature is reduced to 750-850 ℃; and (3) keeping TEAL closed, opening TEGa, and growing a beta-Ga 2O3 film 5 on the (Al x3Ga1-x3)2O3 buffer layer 4) by using an MOCVD process at the temperature of 750-850 ℃, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled at 35-45Torr, the TEGa flow is 45-55sccm, and the growth time is 55-65min.
For example, on the basis of step 4, firstly closing the TEAl and TEGa flow, keeping other growth parameters unchanged, raising the growth temperature to 900 ℃ for thermal annealing for 30min, then keeping other growth parameters unchanged, reducing the growth temperature to 800 ℃, finally keeping the TEAl flow closed, opening the TEGa flow with the flow of 50sccm, and growing the beta-Ga 2O3 film for 60 min.
Preferably, T 4 is 750-850 ℃.
In the invention, the sapphire substrate is c-plane Al 2O3, and Al and Ga belong to the same group element, and the combination mode of the Al and Ga with O atoms is the same, so that the stability of the lattice structure is facilitated. The (Al x1Ga1-x1)2O3 buffer layer, (Al x2Ga1-x2)2O3 buffer layer) and (Al x3Ga1-x3)2O3 buffer layer) of the invention realize element transition between the sapphire substrate and the epitaxial beta-Ga 2O3 film.
According to the invention, the (Al x1Ga1-x1)2O3 buffer layer, (Al x2Ga1-x2)2O3 buffer layer and the (Al x3Ga1-x3)2O3 buffer layer) are sequentially arranged between the beta-Ga 2O3 film and the sapphire substrate from top to bottom, and the (Al x1Ga1-x1)2O3 buffer layer, (Al x2Ga1-x2)2O3 buffer layer) is gradually increased in growth temperature and x1 > x2 > x3 of the Al x3Ga1-x3)2O3 buffer layer, so that the purpose is that the beta-Ga 2O3 film is of a monoclinic system structure, the sapphire substrate is of a corundum structure, the proper epitaxial temperature of the beta-Ga 2O3 film is higher than that of the Al 2O3, and the growth temperature is gradually increased along with the gradual increase of Ga element in the buffer layer, so that each epitaxial film can reach good crystallization quality, and the crystal lattice structure can be gradually transited from the corundum structure of the substrate to the monoclinic system structure of the beta-Ga 2O3 film.
In the present invention (Al x1Ga1-x1)2O3 buffer layer, (Al x2Ga1-x2)2O3 buffer layer and (Al x3Ga1-x3)2O3 buffer layer, x1 > x2 > x 3), and x1 is 0.7-0.9, x2 is 0.4-0.6, x3 is 0.1-0.3, thus making the epitaxial layer also transition to beta-Ga 2O3 film step by step.
According to the invention, a variable-temperature growth (Al 1-xGax)2O3 buffer layer) is introduced between the beta-Ga 2O3 film and the sapphire substrate in the traditional growth process, and because of different lattice structures between the beta-Ga 2O3 film and the sapphire substrate, the introduction of the Al 1-xGax)2O3 buffer layer not only realizes uniform transition of element components between the substrates, but also realizes transition of the lattice structures, thereby reducing dislocation caused by lattice mismatch.
Example two
The present embodiment provides a growth method for manufacturing a beta-Ga 2O3 film using 3min (Al 1-xGax)2O3 buffer layer) on the basis of the above embodiment.
Step 1, placing a sapphire substrate into a solution with an HF acid content of 30% to soak for 60 seconds, then washing with alcohol and acetone, then washing with flowing deionized water, and finally drying with high-purity nitrogen.
And 2, epitaxially growing an (Al 0.8Ga0.2)2O3 buffer layer) for 3 min.
Specifically, the cleaned sapphire substrate was placed in a low-pressure MOCVD reaction chamber, high purity O 2 was used as an O source, TEGa and TEAl were used as a Ga source and an Al source, the reaction chamber temperature was set to 500 ℃, the growth pressure was 40torr, the TEGa flow rate was 10sccm, the TEAl flow rate was 40sccm, the O 2 flow rate was 2100sccm, and an (Al 0.8Ga0.2)2O3 buffer layer) was epitaxially grown on the sapphire substrate for 3 min.
And step3, increasing the growth temperature.
Specifically, other growth parameters are kept unchanged, the Ga source and Al source flow are closed, the heating power of MOCVD is adjusted, and the growth temperature is increased to 600 ℃.
And 4, epitaxially growing an (Al 0.5Ga0.5)2O3 buffer layer) for 3 min.
Specifically, the other growth parameters were kept unchanged, the Ga source and the Al source were turned on at a flow rate of 25sccm, and epitaxially grown for 3min (Al 0.5Ga0.5)2O3 buffer layer).
And step 5, continuously increasing the growth temperature.
Specifically, other growth parameters are kept unchanged, the Ga source and Al source flow are closed, the heating power of MOCVD is adjusted, and the growth temperature is continuously increased to 700 ℃.
And step 6, epitaxially growing an (Al 0.2Ga0.8)2O3 buffer layer) for 3 min.
Specifically, the other growth parameters were kept unchanged, the Ga source and the Al source were turned on at a flow rate of 40 and 10sccm, respectively, and epitaxially grown for 3min (Al 0.2Ga0.8)2O3 buffer layer).
And 7, continuously increasing the growth temperature for thermal annealing.
Specifically, other growth parameters are kept unchanged, the Ga source and Al source flows are closed, and the heating power is adjusted to control the temperature to 900 ℃ for thermal annealing for 30min.
And 8, reducing the growth temperature.
Specifically, the growth parameters of step 7 are kept unchanged, and the heating power control temperature is adjusted to 800 ℃.
And 9, epitaxially growing a beta-Ga 2O3 film for 60 minutes.
Specifically, the Al source is kept closed, the Ga source is opened, the flow is 40sccm, and the beta-Ga 2O3 film is epitaxially grown for 60 minutes.
In the description of the present invention, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying 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 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 point 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 characteristic data points 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.
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 (10)
1. The growth method of the beta-Ga 2O3 film is characterized by comprising the following steps:
Selecting a sapphire substrate (1);
growing (an Al x1Ga1-x1)2O3 buffer layer (2) on the sapphire substrate (1) under the temperature condition of T 1;
Growing (Al x2Ga1-x2)2O3 buffer layer (3) on the (Al x1Ga1-x1)2O3 buffer layer (2) under the temperature condition of T 2;
Growing (Al x3Ga1-x3)2O3 buffer layer (4) on the (Al x2Ga1-x2)2O3 buffer layer (3) under the temperature condition of T 3, wherein x1 > x2 > x3;
A β -Ga 2O3 thin film (5) is grown on the (Al x3Ga1-x3)2O3 buffer layer (4) at a temperature of T 4, wherein T 1＜T2＜T3＜T4.
2. The method of growing a β -Ga 2O3 thin film according to claim 1, characterized in that the sapphire substrate (1) comprises a c-plane sapphire substrate.
3. The method for growing a β -Ga 2O3 thin film according to claim 1, characterized by selecting a sapphire substrate (1) comprising:
and placing the sapphire substrate into an HF acid solution for soaking, then washing the soaked sapphire substrate by using alcohol and acetone, then washing the washed sapphire substrate by using flowing deionized water, and finally drying the washed sapphire substrate by using high-purity nitrogen.
4. The method for growing a β -Ga 2O3 film according to claim 1, wherein T 1 is 450-550 ℃, T 2 is 550-650 ℃, T 3 is 650-750 ℃, and T 4 is 750-850 ℃.
5. The method of growing a β -Ga 2O3 thin film according to claim 4, characterized in that growing (Al x1Ga1-x1)2O3 buffer layer (2) on the sapphire substrate (1) under the temperature condition of T 1, comprising:
And growing the (Al x1Ga1-x1)2O3 buffer layer (2) on the sapphire substrate (1) by utilizing an MOCVD process at the temperature of 450-550 ℃, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled at 35-45Torr, the TEAL flow is 38-42sccm, the TEGa flow is 8-12sccm, and the growth time is 3-5min.
6. The growth method of β -Ga 2O3 thin film according to claim 5, characterized in that (Al x2Ga1-x2)2O3 buffer layer (3) is grown on the (Al x1Ga1-x1)2O3 buffer layer (2) under the condition of T 2 temperature, comprising:
closing TEAL and TEGa, and raising the temperature to 550-650 ℃;
And opening TEAL and TEGa, and growing the (Al x2Ga1-x2)2O3 buffer layer (3) on the (Al x1Ga1-x1)2O3 buffer layer (2) by using an MOCVD process at the temperature of 550-650 ℃, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled at 35-45Torr, the TEAL flow is 22-28sccm, the TEGa flow is 22-28sccm, and the growth time is 3-5min.
7. The growth method of β -Ga 2O3 thin film according to claim 6, characterized in that the growth (Al x3Ga1-x3)2O3 buffer layer (4) is performed on the (Al x2Ga1-x2)2O3 buffer layer (3) under the temperature condition of T 3, comprising:
Closing TEAL and TEGa, and increasing the temperature to 650-750 ℃;
And opening TEAL and TEGa, and growing the (Al x3Ga1-x3)2O3 buffer layer (4) on the (Al x2Ga1-x2)2O3 buffer layer (3) by using an MOCVD process at the temperature of 650-750 ℃, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled at 35-45Torr, the TEAL flow is 8-12sccm, the TEGa flow is 38-42sccm, and the growth time is 3-5min.
8. The method of growing a β -Ga 2O3 thin film according to claim 7, wherein growing a β -Ga 2O3 thin film (5) on the (Al x3Ga1-x3)2O3 buffer layer (4) under the condition of T 4 temperature, comprises:
Closing TEAL and TEGa, heating to 900-950 ℃ for 25-35min, and then reducing the temperature to 750-850 ℃;
And (3) keeping TEAL closed, opening TEGa, and growing the beta-Ga 2O3 film (5) on the (Al x3Ga1-x3)2O3 buffer layer (4) by using an MOCVD process at the temperature of 750-850 ℃, wherein the oxygen flow is 1900-2200sccm, the nitrogen flow is 1000-1200sccm, the growth pressure is controlled at 35-45Torr, the TEGa flow is 45-55sccm, and the growth time is 55-65min.
9. The method for growing a β -Ga 2O3 thin film according to claim 1, wherein x1 is 0.7 to 0.9, x2 is 0.4 to 0.6, and x3 is 0.1 to 0.3.
10. The method for growing a β -Ga 2O3 thin film according to claim 1, wherein the thickness of the (Al x1Ga1-x1)2O3 buffer layer (2), the (Al x2Ga1-x2)2O3 buffer layer (3) and the (Al x3Ga1-x3)2O3 buffer layer (4)) ranges from 30 to 50nm.
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