CN117577516A - Method for growing magnesium-doped gallium oxide film on magnesium oxide substrate - Google Patents
Method for growing magnesium-doped gallium oxide film on magnesium oxide substrate Download PDFInfo
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- CN117577516A CN117577516A CN202311477729.3A CN202311477729A CN117577516A CN 117577516 A CN117577516 A CN 117577516A CN 202311477729 A CN202311477729 A CN 202311477729A CN 117577516 A CN117577516 A CN 117577516A
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- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 49
- 239000000758 substrate Substances 0.000 title claims abstract description 47
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 46
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 27
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000001301 oxygen Substances 0.000 claims abstract description 35
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 35
- 238000009832 plasma treatment Methods 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 230000008021 deposition Effects 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 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 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 abstract description 16
- 239000013078 crystal Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052749 magnesium Inorganic materials 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 238000000861 blow drying Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 26
- 239000010409 thin film Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001451 molecular beam epitaxy Methods 0.000 description 6
- 238000002128 reflection high energy electron diffraction Methods 0.000 description 5
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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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
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02422—Non-crystalline insulating materials, e.g. glass, polymers
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- 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
- H01L21/02367—Substrates
- H01L21/02433—Crystal orientation
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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
- H01L21/02518—Deposited layers
- H01L21/0257—Doping during depositing
- H01L21/02573—Conductivity type
- H01L21/02579—P-type
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- 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
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02656—Special treatments
- H01L21/02658—Pretreatments
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Abstract
A method for growing magnesium doped gallium oxide film on magnesium oxide substrate comprises 1) cleaning magnesium oxide (100) substrate, blow-drying with nitrogen, transferring into molecular beam epitaxial growth system, and performing oxygen plasma treatment; 2) And synchronously carrying out gallium atomic deposition and oxygen plasma treatment on the magnesium oxide (100) substrate subjected to the oxygen plasma treatment to grow a gallium oxide film, wherein the temperature of an operating table is 550-600 ℃. According to the invention, the gallium oxide film grows on the magnesium oxide (100) substrate, the characteristic that the gallium oxide film is matched with the crystal lattice constant of the gallium oxide material is utilized, the characteristic that Mg atoms in the magnesium oxide substrate are very active at high temperature is creatively utilized, the Mg-doped gallium oxide with high crystal epitaxial quality is prepared on the magnesium oxide substrate through simple procedures on the basis of no external Mg source and only by the diffusion of the Mg atoms in the substrate, and a feasible scheme is provided for the p-type preparation of the gallium oxide semiconductor material.
Description
Technical Field
The invention relates to the field of preparation of film materials, in particular to a method for growing a magnesium-doped gallium oxide semiconductor material on a magnesium oxide substrate under the condition of no external magnesium source.
Background
Gallium oxide, which is a third generation wide bandgap semiconductor, has characteristics such as high transmittance from ultraviolet-visible-near infrared region, and can be widely used in transparent electronic devices, deep ultraviolet photodetectors, and high power devices. As a result, more and more researchers are working to produce high quality gallium oxide epitaxial films. Although there have been many reports of successful growth of n-type beta-Ga with good crystal quality and high conductivity 2 O 3 Thin film, but p-type beta-Ga 2 O 3 Films have been rarely reported. Preliminary studies have shown that p-type doping can be performed by doping elements such as Mg. But due to the lack of a reliable preparation method, the lack of a proper dopant, a self-compensation effect and the like, the p-type Mg doped beta-Ga with high quality is obtained 2 O 3 Thin films have been a challenge, and thus growing heteroepitaxially Mg-doped beta-Ga 2 O 3 The monocrystalline film has high application value.
Up to now, many efforts have been made to prepare p-type gallium oxide by Mg doping. In 2017, qian et al deposited a layer of magnesium-doped gallium oxide film on a sapphire substrate by using a magnetron sputtering technology and using a tube furnace after annealing for 4 hours in an argon atmosphere, but the sample crystal prepared by the method has low quality and surface quality, and the preparation method needs two working procedures and is carried out on different equipment, so that the relative complexity is high.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provide a method for growing a high-quality magnesium-doped gallium oxide film on a magnesium oxide substrate, which is simple and does not need an external magnesium source.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for growing a magnesium-doped gallium oxide film on a magnesium oxide substrate comprises the following steps:
1) Cleaning a magnesium oxide (100) substrate, drying with nitrogen, transferring into a molecular beam epitaxial growth system, and performing oxygen plasma treatment;
2) And (2) synchronously carrying out gallium atom deposition and oxygen plasma treatment on the magnesium oxide (100) substrate subjected to the oxygen plasma treatment in the step (1) to grow a gallium oxide film, wherein the temperature of an operating table is 550-600 ℃.
In the step 1), the cleaning can be sequentially performed through ultrasonic cleaning by acetone, alcohol and deionized water.
In the step 1), the oxygen plasma treatment is performed at a high temperature of 0.5 to l.5 hours at a temperature of 550 to 600 ℃ in an operating table.
In the step 1), the oxygen radio frequency power of the oxygen plasma treatment is 230-250W.
In step 1), the oxygen plasma treatment had an oxygen pressure of 4X 10 -5 ～5×10 -5 mbar。
In the step 2), the temperature interval of the gallium source is set to 800-850 ℃.
In the step 2), the gallium atom deposition time is 1-2 h.
In the step 2), the oxygen radio frequency power of the oxygen plasma treatment is 230-250W.
In step 2), the oxygen plasma treatment had an oxygen pressure of 3.5X10 -5 ～4.5×10 -5 mbar。
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
1. the invention adopts molecular beam epitaxy growth equipment (MBE) to prepare high-quality magnesium-doped gallium oxide single crystal film samples on the magnesium oxide substrate, obtains the high-quality magnesium-doped gallium oxide single crystal film through a substrate surface pretreatment process, can be applied to the preparation of solar blind area ultraviolet photoelectric detectors, has great application prospect, and has simple process, good repeatability and certain economic value.
2. According to the invention, the magnesium oxide crystal is in a cubic structure, the magnesium oxide (100) substrate is selected to grow the gallium oxide film, the characteristic that the magnesium oxide film is matched with the crystal lattice constant of the gallium oxide material crystal is utilized, the characteristic that Mg atoms in the magnesium oxide substrate are very active at high temperature is creatively utilized, the Mg-doped gallium oxide with high crystal epitaxial quality is prepared on the magnesium oxide substrate through simple procedures on the basis of no external Mg source only by virtue of the diffusion of the Mg atoms in the substrate, and a feasible scheme is provided for the p-type preparation of the gallium oxide semiconductor material.
3. The invention combines the molecular beam epitaxy method, the substrate selection, the reaction parameter regulation and the like to grow the magnesium doped gallium oxide film, and the magnesium is passively doped to the gallium oxide, thereby obtaining the wide forbidden band of 5.14eV. The molecular beam epitaxy method of the invention utilizes the active characteristic of Mg atoms of the substrate at high temperature to prepare the magnesium-doped gallium oxide film, and is characterized in that the selection of substrate materials and the selection of proper crystal faces of the substrate are adopted; in the process of growing thin films on the magnesium oxide (100) surface, the key is the choice of parameters for the stage temperature and oxygen pressure.
4. The invention utilizes molecular beam epitaxy equipment to perform oxygen plasma treatment on the magnesium oxide substrate, and then directly grows a gallium oxide film on the treated magnesium oxide substrate, thereby simplifying the process flow and preparing the high-quality ultra-wide band-gap magnesium-doped gallium oxide film.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of the magnesium-doped gallium oxide thin films prepared in example 1 and comparative example 1.
FIG. 2 is a reflection high-energy electron diffraction (RHEED) diagram of the magnesium-doped gallium oxide film prepared in example 1.
FIG. 3 is a reflection high-energy electron diffraction (RHEED) diagram of the magnesium-doped gallium oxide film prepared in comparative example 2.
FIG. 4 shows the film (. Alpha.hν) of magnesium-doped gallium oxide obtained in example 1 2 -an hν picture.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear and obvious, the invention is further described in detail below with reference to the accompanying drawings and embodiments.
Example 1
The method for preparing the magnesium-doped gallium oxide film comprises the following steps:
1. a gallium oxide film is grown on a magnesium oxide (100) substrate, and the substrate is a magnesium oxide substrate with the specification of 10mm multiplied by 0.5 mm. Firstly, ultrasonically cleaning a substrate sequentially through acetone, ethanol and deionized water for 5 minutes in a single time, and then drying by nitrogen and transferring the substrate into a growth cavity of a molecular beam epitaxy system.
2. High temperature treatment of oxygen plasma at 600deg.C for 1 hr with RF power of 250W and oxygen pressure of 5×10 -5 The substrate can be cleaned and the generation of oxygen vacancy defects of the substrate can be restrained by selecting the treatment under the high-temperature oxygen atmosphere.
3. At an oxygen pressure of 4X 10 -5 Growing a gallium oxide film for 1h in an oxygen atmosphere of mbar, wherein the temperature interval of a gallium source is set to 800-850 ℃, the temperature of an operating table is 600 ℃, and the radio frequency power is 240W. The sample prepared was labeled GM-600.
Comparative example 1
The method for producing a gallium oxide thin film of this comparative example is different from example 1 in that the stage temperature in step (3) is 400 ℃. The sample prepared was labeled GM-400.
Comparative example 2
The method for preparing a gallium oxide thin film of this comparative example is different from example 1 in that the substrate selected is magnesium oxide (110). The prepared sample was labeled GM- (110).
FIG. 1 is a graph of a sample characterization by an X-Ray diffractometer showing that the epitaxial relationship of the film to the substrate is beta-Ga 2 O 3 (100) /(MgO) (100). It can be seen that the peak intensity of the GM-400 sample was significantly weaker than that of the GM-600 sample, while the peak width at half maximum of the GM-400 sample was significantly greater than that of the GM-600 sample. These two points demonstrate that the crystal quality of sample GM-600 prepared at 600℃bench temperature is significantly higher than that of GM-400 prepared at 400 ℃.
FIG. 2 is a RHEED view of a GM-600 film characterized by a reflective high energy electron diffractometer, showing a continuous sharp striped spot, showing a very good surface flatness and regular periodic atomic arrangement of the grown gallium oxide film.
FIG. 3 is a RHEED view of a GM- (110) thin film characterized by a reflective high-energy electron diffractometer, and shows discontinuous punctiform light spots, which indicate poor surface quality and crystal quality of the grown gallium oxide thin film, and a significant difference from the RHEED view obtained by the GM-600 thin film in FIG. 2.
FIG. 4 is a sample of GM-600 (. Alpha.hν) 2 And (3) extrapolating the straight line part to the axis of abscissa by the h v curve, wherein the intersection point is the forbidden bandwidth of the sample, and the forbidden bandwidth of the sample is 5.14eV. GM-600 has a wide band gap of 5.14eV due to high concentration of Mg doping.
Claims (9)
1. The method for growing the magnesium-doped gallium oxide film on the magnesium oxide substrate is characterized by comprising the following steps of:
1) Cleaning a magnesium oxide (100) substrate, drying with nitrogen, transferring into a molecular beam epitaxial growth system, and performing oxygen plasma treatment;
2) And (2) synchronously carrying out gallium atom deposition and oxygen plasma treatment on the magnesium oxide (100) substrate subjected to the oxygen plasma treatment in the step (1) to grow a gallium oxide film, wherein the temperature of an operating table is 550-600 ℃.
2. A method for growing a magnesium-doped gallium oxide film on a magnesium oxide substrate according to claim 1, wherein: in the step 1), the cleaning can be sequentially performed through ultrasonic cleaning by acetone, alcohol and deionized water.
3. A method for growing a magnesium-doped gallium oxide film on a magnesium oxide substrate according to claim 1, wherein: in the step 1), the oxygen plasma treatment is performed at a high temperature of 0.5 to l.5 hours at a temperature of 550 to 600 ℃ in an operating table.
4. A method for growing a magnesium-doped gallium oxide film on a magnesium oxide substrate according to claim 1, wherein: in the step 1), the oxygen radio frequency power of the oxygen plasma treatment is 230-250W.
5. A method for growing a magnesium-doped gallium oxide film on a magnesium oxide substrate according to claim 1, wherein: in step 1), the oxygen plasma treatment had an oxygen pressure of 4X 10 -5 ～5×10 -5 mbar。
6. A method for growing a magnesium-doped gallium oxide film on a magnesium oxide substrate according to claim 1, wherein: in the step 2), the temperature interval of the gallium source is set to 800-850 ℃.
7. A method for growing a magnesium-doped gallium oxide film on a magnesium oxide substrate according to claim 1, wherein: in the step 2), the gallium atom deposition time is 1-2 h.
8. A method for growing a magnesium-doped gallium oxide film on a magnesium oxide substrate according to claim 1, wherein: in the step 2), the oxygen radio frequency power of the oxygen plasma treatment is 230-250W.
9. A method for growing a magnesium-doped gallium oxide film on a magnesium oxide substrate according to claim 1, wherein: in step 2), the oxygen plasma treatment had an oxygen pressure of 3.5X10 -5 ～4.5×10 -5 mbar。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311477729.3A CN117577516A (en) | 2023-11-07 | 2023-11-07 | Method for growing magnesium-doped gallium oxide film on magnesium oxide substrate |
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| CN202311477729.3A CN117577516A (en) | 2023-11-07 | 2023-11-07 | Method for growing magnesium-doped gallium oxide film on magnesium oxide substrate |
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