CN114855269B - Method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate and molecular beam epitaxy equipment - Google Patents
Method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate and molecular beam epitaxy equipment Download PDFInfo
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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 182
- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 182
- 239000000758 substrate Substances 0.000 title claims abstract description 107
- 238000001451 molecular beam epitaxy Methods 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 35
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 98
- 239000010935 stainless steel Substances 0.000 claims abstract description 98
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 57
- 239000001301 oxygen Substances 0.000 claims description 57
- 229910052760 oxygen Inorganic materials 0.000 claims description 57
- 238000001883 metal evaporation Methods 0.000 claims description 52
- 229910052751 metal Inorganic materials 0.000 claims description 45
- 239000002184 metal Substances 0.000 claims description 45
- 238000002347 injection Methods 0.000 claims description 28
- 239000007924 injection Substances 0.000 claims description 28
- 238000001704 evaporation Methods 0.000 claims description 19
- 230000008020 evaporation Effects 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000012544 monitoring process Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000004093 laser heating Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 106
- 230000001276 controlling effect Effects 0.000 description 5
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- 230000001105 regulatory effect Effects 0.000 description 3
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 2
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- RYYVLZVUVIJVGH-UHFFFAOYSA-N trimethylxanthine Natural products CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 1
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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Abstract
The invention provides a method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate and a molecular beam epitaxy device, wherein the molecular beam epitaxy device comprises an MBE growth chamber, a stainless steel tray arranged in the MBE growth chamber and the high-resistance gallium oxide substrate arranged at the bottom end of the stainless steel tray. In the invention, as the absorption of the high-resistance gallium oxide substrate to the laser is very small, the laser can directly irradiate the stainless steel tray through the high-resistance gallium oxide substrate, so that the stainless steel tray in the MBE growth chamber can be uniformly heated in a laser heating mode through the laser arranged at the bottom end of the stainless steel tray, and further the uniform heating of the high-resistance gallium oxide substrate is realized, and the homoepitaxial gallium oxide film with high quality and uniform thickness is prepared.
Description
Technical Field
The invention relates to the technical field of gallium oxide film preparation, in particular to a method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate and a molecular beam epitaxy device.
Technical Field
Gallium oxide (Ga) 2 O 3 ) As an emerging third generation wide bandgap semiconductor, the semiconductor has the advantages of ultra-wide bandgap, high breakdown field strength and the like. The transparent oxide semiconductor material has excellent physical and chemical characteristics, good electrical conductivity and luminous performance, and has wide application prospect in the fields of power semiconductor devices, ultraviolet detectors, gas sensors and optoelectronic devices. Gallium oxide has a 5-crystal structure, which is respectively rhombohedral (α), monoclinic (β), defective spinel (γ), cubic (δ), and orthorhombic (ε). beta-Ga 2 O 3 Because of the stability at high temperature, it is becoming a research hot spot in recent years at home and abroad, and it is not specifically described that the gallium oxide mentioned below refers to beta-Ga 2 O 3 。
In the epitaxial method of gallium oxide, molecular Beam Epitaxy (MBE) is one of the main means for growing high-purity and high-quality gallium oxide epitaxial films, and by utilizing ultrahigh vacuum and high-purity source materials, the concentration of unintentionally doped impurities can be effectively reduced, and the accurate regulation and control of the atomic scale growth can be realized. The gallium oxide film epitaxially grown by MBE has the advantages of good crystal quality, flat surface and controllable electron concentration, which are necessary conditions for obtaining high-performance gallium oxide-based power electronic devices and photoelectric conversion devices. Therefore, a layer of unintentionally doped gallium oxide buffer layer film and a layer of AlGaO film can be sequentially homoepitaxial on the high-resistance gallium oxide substrate by MBE by using equipment and used for preparing a High Electron Mobility Transistor (HEMT) device.
Aiming at the technical characteristics of the existing MBE, in the process of preparing the gallium oxide homoepitaxial film by using MBE equipment, the gallium oxide substrate needs to be maintained in a high-temperature state suitable for the growth of the gallium oxide film. In the prior art, the gallium oxide substrate is heated by heat radiation through a heating wire arranged behind the substrate. Due to the fact that certain space distribution exists in the arrangement of the heating wires, the heating of the substrate is uneven, the quality and thickness uniformity of the prepared epitaxial wafer are seriously affected, and even the epitaxial layer is cracked.
Accordingly, the prior art is still in need of improvement and development.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate and a molecular beam epitaxy device, which aim to solve the problem that the quality and thickness uniformity of a gallium oxide epitaxial wafer prepared on a high-resistance gallium oxide substrate in the prior art are poor.
The technical scheme of the invention is as follows:
the molecular beam epitaxy equipment for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises an MBE growth chamber, a stainless steel tray arranged in the MBE growth chamber and the high-resistance gallium oxide substrate arranged at the bottom end of the stainless steel tray, wherein a laser is arranged below the stainless steel tray, and a laser spot emitted by the laser covers the whole bottom end of the stainless steel tray.
The molecular beam epitaxy equipment for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate is characterized in that a beam expander is arranged on the laser.
The molecular beam epitaxy device for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate is characterized in that the laser emitted by the laser has the wavelength of 500-1500nm.
A method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate based on molecular beam epitaxy equipment comprises the following steps:
a molecular pump is started in advance to vacuumize the MBE growth chamber;
fixing an unintended doped gallium oxide substrate at the bottom end of a stainless steel tray, and enabling the growth surface of the unintended doped gallium oxide substrate to face downwards;
stopping a molecular pump, filling nitrogen into a rapid sample injection cavity, and then, placing the stainless steel tray fixed with the unintended doped gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of a Ga metal evaporation source and an Al metal doping source, and setting the rapid flow intensity of the Ga metal evaporation source and the Al metal doping source when the Ga metal evaporation source and the Al metal doping source reach the preset evaporation temperature;
starting a molecular pump, vacuumizing the rapid sample injection cavity, and when the vacuum degree of the rapid sample injection cavity is lower than 10 - 8 At mbar, transferring the stainless steel tray fixed with the unintended doped gallium oxide substrate into the MBE growth chamber, and opening the laser to heat the stainless steel tray;
slowly opening an oxygen plasma source pipeline angle valve, and setting the oxygen flow to be 0.1-0.5sccm on a digital flowmeter;
after the laser heats the stainless steel tray to a preset film growth temperature, an oxygen source is started, oxygen plasma is lightened, the oxygen pressure is waited to be stable, a baffle of the Ga metal evaporation source is controlled to be set in an automatic mode, and the unintended homoepitaxial growth of the gallium oxide doped film is carried out;
monitoring that the unintended doped gallium oxide film is homoepitaxially grown to a first preset thickness, maintaining the supply of an oxygen source and a Ga metal evaporation source, setting a baffle control of an Al metal doping source as an automatic mode, and continuing to grow an AlGaO epitaxial film on the unintended doped gallium oxide film;
and after the AlGaO epitaxial film grows to a second preset thickness, the baffle plates of the Ga metal evaporation source and the Al metal doping source are automatically closed, the oxygen source supply is kept, the cooling rate of the stainless steel tray is set to be 5-35 ℃/min, when the temperature of the stainless steel tray is lower than 200 ℃, the oxygen source is cut off, the laser is closed, and the preparation of the unintended doped gallium oxide film and the AlGaO epitaxial film on the high-resistance substrate is completed.
The method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate comprises pre-starting a molecular pump to vacuumize MBE growth chamber, and vacuumizing the MBE growth chamber to below 2×10 -9 mbar。
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises the steps of presetting the evaporation temperature of 1000-1200 ℃ and the heating rate of 2-10 ℃/min of a Ga metal evaporation source and an Al metal doping source.
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises the steps of enabling the rapid flow intensity of the Ga metal evaporation source and the Al metal doping source to be 1 multiplied by 10 -8 -9×10 -7 mbar。
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises the step of heating the stainless steel tray to a preset film growth temperature by the laser, wherein the preset film growth temperature is 600-1000 ℃, and the heating rate is 5-15 ℃/min.
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises the steps of enabling the homoepitaxial growth speed of the unintended doped gallium oxide film to be 10-100 nanometers/hour, and enabling the first preset thickness to be 100-500 nanometers.
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises the steps of growing the AlGaO epitaxial film at a speed of 10-50 nanometers/hour and a second preset thickness of 10-60 nanometers.
The beneficial effects are that: the invention provides a method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate and molecular beam epitaxy equipment. In the invention, as the absorption of the high-resistance gallium oxide substrate to the laser is very small, the laser can directly irradiate the stainless steel tray through the high-resistance gallium oxide substrate, so that the stainless steel tray in the MBE growth chamber can be uniformly heated in a laser heating mode through the laser arranged at the bottom end of the stainless steel tray, and further the high-resistance gallium oxide substrate is uniformly heated, and the homoepitaxial gallium oxide film with high quality and uniform thickness is prepared.
Drawings
Fig. 1 is a schematic diagram of a molecular beam epitaxy apparatus for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate according to the present invention.
Fig. 2 is a graph of laser transmittance for an annealed and unannealed Fe-doped (high-resistance) gallium oxide substrate.
Fig. 3 is a flow chart of a method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate.
Detailed Description
The invention provides a method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate and a molecular beam epitaxy device, and the invention is further described in detail below in order to make the purposes, technical schemes and effects of the invention clearer and more definite. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Since it is necessary to maintain the gallium oxide substrate in a high temperature state suitable for the growth of the gallium oxide thin film during the preparation of the gallium oxide homoepitaxial thin film using the molecular beam epitaxy apparatus. The heating mode of the gallium oxide substrate in the existing molecular beam epitaxy equipment can lead to uneven heating of the substrate, thereby seriously affecting the quality and thickness uniformity of the epitaxial wafer and even leading to cracking of the epitaxial wafer.
Based on this, the present invention provides a molecular beam epitaxy apparatus for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate, as shown in fig. 1, which includes an MBE growth chamber 10, a stainless steel tray 20 disposed in the MBE growth chamber 10, and a high-resistance gallium oxide substrate 30 disposed at the bottom end of the stainless steel tray 20, wherein a laser 40 is disposed below the stainless steel tray 20, and a laser spot emitted by the laser 40 covers the entire bottom end of the stainless steel tray 20.
Specifically, it is reported in the literature that the high-resistance gallium oxide substrate has a high transmittance in the infrared band, mainly because of the weak reflection of electrons by plasma, as shown in FIG. 2 (data from SCI paper: structural and electronic characteristics of Fe-doped beta-Ga 2O3single crystals and the annealing effects). That is, since the absorption of infrared laser light by the high-resistance gallium oxide substrate is extremely small, laser light directly irradiated on the high-resistance gallium oxide substrate can be directly transmitted while being irradiated on the stainless steel tray in the process of heating the high-resistance gallium oxide substrate using laser light of a usual infrared band. Therefore, the embodiment can uniformly heat the stainless steel tray in the MBE growth chamber in a laser heating mode through the laser arranged above the stainless steel tray, so that the high-resistance gallium oxide substrate is uniformly heated, and the homoepitaxial gallium oxide film with high quality and uniform thickness is prepared and is used for preparing High Electron Mobility Transistor (HEMT) devices.
In some embodiments, at least 1 laser is disposed above the stainless steel tray. As an example, 2 lasers may be provided above the stainless steel tray; 3, 4, 5, 6, etc. may be provided. When setting up 2 or more than 2 lasers, only need guarantee that the laser that a plurality of lasers sent can evenly cover the bottom of stainless steel tray.
In some embodiments, a beam expander is disposed on the laser. In this embodiment, the beam expander is disposed on the laser, so that the spot size of the laser can be adjusted, and the laser spot can cover the top of the whole stainless steel tray.
In some embodiments, the laser emits laser light having a wavelength of 500-1500nm. Preferably, the laser emits laser light with a wavelength of 800-1200nm. By way of example, the laser emits laser wavelengths of 800nm, 900nm, 1000nm, 1200nm, etc.
In some embodiments, there is also provided a method for preparing a homoepitaxial gallium oxide thin film on a high-resistance gallium oxide substrate based on a molecular beam epitaxy apparatus, as shown in fig. 3, comprising the steps of:
s10, starting a molecular pump in advance to vacuumize the MBE growth chamber;
s20, fixing an unintended doped gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the unintended doped gallium oxide substrate faces downwards;
s30, stopping the molecular pump, filling nitrogen into the rapid sample injection cavity to break vacuum, and then placing the stainless steel tray fixed with the unintended doped gallium oxide substrate into the rapid sample injection cavity;
s40, setting the evaporation temperature of a Ga metal evaporation source and an Al metal doping source, and setting the rapid flow intensity of the Ga metal evaporation source and the Al metal doping source when the Ga metal evaporation source and the Al metal doping source reach the preset evaporation temperature;
s50, starting a molecular pump, vacuumizing the rapid sample injection cavity, and when the vacuum degree of the rapid sample injection cavity is lower than 10 -8 At mbar, transferring the stainless steel tray fixed with the unintended doped gallium oxide substrate into the MBE growth chamber, and opening the laser to heat the stainless steel tray;
s60, slowly opening an oxygen plasma source pipeline angle valve, and setting the oxygen flow to be 0.1-0.5sccm on a digital flowmeter;
s70, after the laser heats the stainless steel tray to a preset film growth temperature, starting an oxygen source, igniting oxygen plasma, waiting for stable oxygen pressure, setting a baffle control of a Ga metal evaporation source to be an automatic mode, and carrying out the homoepitaxial growth of the unintended doped gallium oxide film;
s80, monitoring that after the unintended doped gallium oxide film is homoepitaxially grown to a first preset thickness, keeping the supply of an oxygen source and a Ga metal evaporation source, setting the baffle control of an Al metal doping source as an automatic mode, and continuing to grow an AlGaO epitaxial film on the unintended doped gallium oxide film;
and S90, after the AlGaO epitaxial film grows to a second preset thickness, the Ga metal evaporation source and the baffle of the Al metal doping source are automatically closed, the oxygen source supply is kept, the cooling rate of the stainless steel tray is set to be 5-35 ℃/min, when the temperature of the stainless steel tray is lower than 200 ℃, the oxygen source is cut off, the laser is closed, and the preparation of the unintended doped gallium oxide film and the AlGaO epitaxial film on the high-resistance substrate is completed.
In the embodiment, the heating temperature of the stainless steel tray can be adjusted by controlling the power of the laser, so that the heating temperature of the high-resistance gallium oxide substrate is adjusted; the growth speed of the homoepitaxial gallium oxide film can be controlled by adjusting the fast flow intensity of the Ga metal evaporation source and the Al metal doping source and the flow rate of the oxygen source. In the process of preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate, the stainless steel tray is uniformly heated under the irradiation of laser, so that the high-resistance gallium oxide substrate is uniformly heated. Meanwhile, the temperature of the high-resistance gallium oxide substrate is measured in real time through the temperature sensor and fed back to the laser, so that the laser output power is adjusted, and the temperature of the high-resistance gallium oxide substrate is maintained in a temperature range suitable for gallium oxide epitaxial growth.
According to the embodiment, the stainless steel tray in the growth chamber of the molecular beam epitaxy equipment is uniformly heated by a laser heating method, so that the high-resistance gallium oxide substrate is uniformly heated, and a high-quality and uniform-thickness unintentional doped gallium oxide film buffer layer and a weak-conductivity gallium oxide film (AlGaO epitaxy film) are prepared and are used for preparing High Electron Mobility Transistor (HEMT) devices.
In some embodiments, the step of evacuating the MBE growth chamber by pre-activating the molecular pumpThe MBE growth chamber is vacuumized to be lower than 2 multiplied by 10 -9 mbar。
In some embodiments, the preset evaporation temperature of the Ga metal evaporation source and the Al metal doping source is 1000-1200 ℃, and the heating rate is 2-10 ℃/min, but is not limited thereto.
In some embodiments, the Ga metal evaporation source and the Al metal doping source have a fast flow intensity of 1X 10 -8 -9×10 -7 mbar, but is not limited thereto.
In some embodiments, the laser heats the stainless steel tray to a preset film growth temperature of 600-1000 ℃ at a heating rate of 5-15 ℃/min, but is not limited thereto.
In some embodiments, the unintentional doped gallium oxide thin film homoepitaxially grows at a rate of 10-100 nanometers per hour and a first preset thickness of 100-500nm; the growth speed of the AlGaO epitaxial film is 10-50 nanometers/hour, and the second preset thickness is 10-60 nanometers.
The invention is further illustrated by the following examples:
example 1
A method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate based on a molecular beam epitaxy device, wherein the molecular beam epitaxy device comprises an MBE growth chamber, a stainless steel tray arranged in the MBE growth chamber and a high-resistance gallium oxide substrate arranged at the bottom end of the stainless steel tray, 1 laser is arranged below the stainless steel tray, and a laser spot emitted by the laser covers the whole bottom end of the stainless steel tray; the method comprises the following steps:
confirming that water, electricity and gas of MBE equipment are normally supplied, and starting a molecular pump in advance to vacuumize an MBE growth chamber until the vacuum degree is lower than 2 multiplied by 10 -9 mbar；
Fixing a 2-inch clean Fe-doped high-resistance gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the unintended doped gallium oxide substrate faces downwards;
stopping a molecular pump, filling nitrogen into a rapid sample injection cavity, and then, placing the stainless steel tray fixed with the unintended doped gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of the Ga metal evaporation source and the Al metal doping source to be 1100 ℃, heating and cooling at a speed of 6 ℃/min, measuring the beam intensity of the Ga metal evaporation source and the Al metal doping source by using a beam gauge when the Ga metal evaporation source and the Al metal doping source reach the preset evaporation temperature of 1100 ℃, and adjusting the temperatures of the Ga metal evaporation source and the Al metal doping source according to the stable beam gauge reading to maintain the beam intensity at 5 multiplied by 10 -7 mbar；
Starting a molecular pump, vacuumizing the rapid sample injection cavity, and when the vacuum degree of the rapid sample injection cavity is lower than 10 - 8 When mbar is carried out, the stainless steel tray fixed with the unintended doped gallium oxide substrate is transferred into the MBE growth chamber, the laser is opened to heat the stainless steel tray, and meanwhile, the temperature of the substrate is measured in real time through the temperature sensor and fed back to the laser, so that the output power of the laser is regulated, and the temperature of the substrate is maintained in a temperature range suitable for epitaxial growth;
slowly opening an oxygen plasma source pipeline angle valve, and setting the oxygen flow to be 0.3sccm on a digital flowmeter;
heating the stainless steel tray to a preset film growth temperature of 800 ℃ by the laser, and then heating at a heating rate of 10 ℃/min; starting an oxygen source, igniting oxygen plasma, waiting for stable oxygen pressure, setting a baffle plate of a Ga metal evaporation source to be in an automatic mode, setting the growth speed to be 60 nanometers/hour, and carrying out the homoepitaxial growth of the unintended doped gallium oxide film;
monitoring that the homoepitaxial growth of the unintended doped gallium oxide film is completed after the homoepitaxial growth of the unintended doped gallium oxide film reaches the thickness of 300 nanometers; maintaining the supply of an oxygen source and a Ga metal evaporation source, setting a baffle control of an Al metal doping source into an automatic mode, setting the growth speed to be 30 nanometers/hour, continuously growing an AlGaO epitaxial film on an unintended doped gallium oxide film, and controlling the doping mole percentage of Al to be not more than 23 percent;
and after the AlGaO epitaxial film grows to 50 nanometers, the baffle plates of the Ga metal evaporation source and the Al metal doping source are automatically closed, the oxygen source supply is kept, the cooling rate of the stainless steel tray is set to 20 ℃/min, when the temperature of the stainless steel tray is lower than 200 ℃, the oxygen source is cut off, and the laser is closed, so that the preparation of the unintended doped gallium oxide film and the AlGaO epitaxial film on the high-resistance substrate is completed.
Example 2
A method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate based on a molecular beam epitaxy device, wherein the molecular beam epitaxy device comprises an MBE growth chamber, a stainless steel tray arranged in the MBE growth chamber and a high-resistance gallium oxide substrate arranged at the bottom end of the stainless steel tray, 1 laser is arranged below the stainless steel tray, and a laser spot emitted by the laser covers the whole bottom end of the stainless steel tray; the method comprises the following steps:
confirming that water, electricity and gas of MBE equipment are normally supplied, and starting a molecular pump in advance to vacuumize an MBE growth chamber until the vacuum degree is lower than 2 multiplied by 10 -9 mbar；
Fixing a 2-inch clean Fe-doped high-resistance gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the unintended doped gallium oxide substrate faces downwards;
stopping a molecular pump, filling nitrogen into a rapid sample injection cavity, and then, placing the stainless steel tray fixed with the unintended doped gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of the Ga metal evaporation source and the Al metal doping source to be 1000 ℃, heating and cooling at a speed of 2 ℃/min, measuring the beam intensity of the Ga metal evaporation source and the Al metal doping source by using a beam gauge when the evaporation temperature of the Ga metal evaporation source and the Al metal doping source reaches the preset evaporation temperature of 1000 ℃, and adjusting the temperatures of the Ga metal evaporation source and the Al metal doping source according to the stable beam gauge reading to maintain the beam intensity at 1 multiplied by 10 -8 mbar；
Starting a molecular pump, vacuumizing the rapid sample injection cavity, and when the vacuum degree of the rapid sample injection cavity is lower than 10 - 8 At mbar, the stainless steel tray fixed with the unintentionally doped gallium oxide substrate is transferred into theIn the MBE growth chamber, the laser is opened to heat the stainless steel tray, and meanwhile, the temperature of the substrate is measured in real time through the temperature sensor and fed back to the laser, so that the laser output power is regulated, and the temperature of the substrate is maintained in a temperature range suitable for epitaxial growth;
slowly opening an oxygen plasma source pipeline angle valve, and setting the oxygen flow to be 0.1-0.5sccm on a digital flowmeter;
after the laser heats the stainless steel tray to a preset film growth temperature of 600 ℃, the heating rate is 5 ℃/min; starting an oxygen source, igniting oxygen plasma, waiting for stable oxygen pressure, setting a baffle plate of a Ga metal evaporation source to be in an automatic mode, setting the growth speed to be 20-100 nanometers/hour, and carrying out the homoepitaxial growth of an unintended doped gallium oxide film;
monitoring that the homoepitaxial growth of the unintended doped gallium oxide film is completed after the homoepitaxial growth of the unintended doped gallium oxide film reaches the thickness of 300 nanometers; maintaining the supply of an oxygen source and a Ga metal evaporation source, setting a baffle control of an Al metal doping source into an automatic mode, setting the growth speed to be 10 nanometers/hour, continuously growing an AlGaO epitaxial film on an unintended doped gallium oxide film, and controlling the doping mole percentage of Al to be not more than 23 percent;
and after the AlGaO epitaxial film grows to 50 nanometers, the baffle plates of the Ga metal evaporation source and the Al metal doping source are automatically closed, the oxygen source supply is kept, the cooling rate of the stainless steel tray is set to 5 ℃/min, when the temperature of the stainless steel tray is lower than 200 ℃, the oxygen source is cut off, and the laser is closed, so that the preparation of the unintended doped gallium oxide film and the AlGaO epitaxial film on the high-resistance substrate is completed.
Example 3
A method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate based on a molecular beam epitaxy device, wherein the molecular beam epitaxy device comprises an MBE growth chamber, a stainless steel tray arranged in the MBE growth chamber and a high-resistance gallium oxide substrate arranged at the bottom end of the stainless steel tray, 1 laser is arranged below the stainless steel tray, and a laser spot emitted by the laser covers the whole bottom end of the stainless steel tray; the method comprises the following steps:
confirming that water, electricity and gas of MBE equipment are normally supplied, and starting a molecular pump in advance to vacuumize an MBE growth chamber until the vacuum degree is lower than 2 multiplied by 10 -9 mbar；
Fixing a 2-inch clean Fe-doped high-resistance gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the unintended doped gallium oxide substrate faces downwards;
stopping a molecular pump, filling nitrogen into a rapid sample injection cavity, and then, placing the stainless steel tray fixed with the unintended doped gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of the Ga metal evaporation source and the Al metal doping source to be 1200 ℃, heating and cooling at a speed of 10 ℃/min, measuring the beam intensity of the Ga metal evaporation source and the Al metal doping source by using a beam gauge when the evaporation temperature of the Ga metal evaporation source and the Al metal doping source reaches the preset evaporation temperature of 1200 ℃, and adjusting the temperatures of the Ga metal evaporation source and the Al metal doping source according to the stable beam gauge reading to maintain the beam intensity at 9 multiplied by 10 -7 mbar；
Starting a molecular pump, vacuumizing the rapid sample injection cavity, and when the vacuum degree of the rapid sample injection cavity is lower than 10 - 8 When mbar is carried out, the stainless steel tray fixed with the unintended doped gallium oxide substrate is transferred into the MBE growth chamber, the laser is opened to heat the stainless steel tray, and meanwhile, the temperature of the substrate is measured in real time through the temperature sensor and fed back to the laser, so that the output power of the laser is regulated, and the temperature of the substrate is maintained in a temperature range suitable for epitaxial growth;
slowly opening an oxygen plasma source pipeline angle valve, and setting the oxygen flow to be 0.5sccm on a digital flowmeter;
after the laser heats the stainless steel tray to a preset film growth temperature of 1000 ℃, the heating rate is 15 ℃/min; starting an oxygen source, igniting oxygen plasma, waiting for stable oxygen pressure, setting a baffle plate of a Ga metal evaporation source to be in an automatic mode, setting the growth speed to be 100 nanometers/hour, and carrying out the homoepitaxial growth of the unintended doped gallium oxide film;
monitoring that the homoepitaxial growth of the unintended doped gallium oxide film is completed after the homoepitaxial growth of the unintended doped gallium oxide film reaches the thickness of 300 nanometers; maintaining the supply of an oxygen source and a Ga metal evaporation source, setting a baffle control of an Al metal doping source into an automatic mode, setting the growth speed to be 50 nanometers/hour, continuously growing an AlGaO epitaxial film on an unintended doped gallium oxide film, and controlling the doping mole percentage of Al to be not more than 23 percent;
and after the AlGaO epitaxial film grows to 50 nanometers, the baffle plates of the Ga metal evaporation source and the Al metal doping source are automatically closed, the oxygen source supply is kept, the cooling rate of the stainless steel tray is set to 35 ℃/min, when the temperature of the stainless steel tray is lower than 200 ℃, the oxygen source is cut off, and the laser is closed, so that the preparation of the unintended doped gallium oxide film and the AlGaO epitaxial film on the high-resistance substrate is completed.
Comparative example 1
A method for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate based on a molecular beam epitaxy device, wherein the molecular beam epitaxy device comprises an MBE growth chamber, a stainless steel tray arranged in the MBE growth chamber and a high-resistance gallium oxide substrate arranged on the stainless steel tray, wherein an induction coil is arranged on the outer side of the MBE growth chamber, and the induction coil is used for heating the stainless steel tray so as to transfer heat to the high-resistance gallium oxide substrate on the stainless steel tray; the method comprises the following steps:
confirming that water, electricity and gas of MBE equipment are normally supplied, and starting a molecular pump in advance to vacuumize an MBE growth chamber until the vacuum degree is lower than 2 multiplied by 10 -9 mbar；
Fixing a 2-inch clean Fe-doped high-resistance gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the unintended doped gallium oxide substrate faces downwards;
stopping a molecular pump, filling nitrogen into a rapid sample injection cavity, and then, placing the stainless steel tray fixed with the unintended doped gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of Ga metal evaporation source and Al metal doping sourceThe temperature is 1100 ℃, the heating and cooling rate is 60 ℃/min, when the Ga metal evaporation source and the Al metal doping source reach the preset evaporation temperature of 1100 ℃, the beam intensity is measured by using a beam gauge, and the temperature of the Ga metal evaporation source and the Al metal doping source is adjusted according to the stable beam gauge reading, so that the beam intensity is maintained to be 1 multiplied by 10 -8 -9×10 -7 mbar；
Starting a molecular pump, vacuumizing the rapid sample injection cavity, and when the vacuum degree of the rapid sample injection cavity is lower than 10 - 8 When mbar is carried out, the stainless steel tray fixed with the unintended doped gallium oxide substrate is transferred into the MBE growth chamber, and an induction coil power supply is started to heat the stainless steel tray, so that the substrate temperature is maintained in a temperature range suitable for epitaxial growth;
slowly opening an oxygen plasma source pipeline angle valve, and setting the oxygen flow to be 0.3sccm on a digital flowmeter;
when the induction coil heats the stainless steel tray to a preset film growth temperature of 800 ℃, an oxygen source is started, oxygen plasma is lightened, the oxygen pressure is kept stable, a baffle of the Ga metal evaporation source is controlled to be set in an automatic mode, the growth speed is controlled to be 60 nanometers/hour, and the homoepitaxial growth of the unintended doped gallium oxide film is carried out;
monitoring that the homoepitaxial growth of the unintended doped gallium oxide film is completed after the homoepitaxial growth of the unintended doped gallium oxide film reaches the thickness of 300 nanometers; maintaining the supply of an oxygen source and a Ga metal evaporation source, setting a baffle control of an Al metal doping source into an automatic mode, setting the growth speed to be 30 nanometers/hour, continuously growing an AlGaO epitaxial film on an unintended doped gallium oxide film, and controlling the doping mole percentage of Al to be not more than 23 percent;
and after the AlGaO epitaxial film grows to 50 nanometers, the baffle plates of the Ga metal evaporation source and the Al metal doping source are automatically closed, the oxygen source supply is kept, the cooling rate of the stainless steel tray is set to 20 ℃/min, when the temperature of the stainless steel tray is lower than 200 ℃, the oxygen source is cut off, the power supply of the induction coil is turned off, and the preparation of the unintended doped gallium oxide film and the AlGaO epitaxial film on the high-resistance substrate is completed.
Example 4
Measurement of the thickness and Standard deviation of thickness of homoepitaxial gallium oxide films prepared in examples 1 to 3 and comparative example 1
After the preparation of the homoepitaxial gallium oxide film on the wafer is finished, 32 points (8 points are distributed at equal intervals in four radial directions, 45-degree angles are formed at equal intervals in the four directions and the circle center is not included) are selected in a Chinese character 'mi' shape on the wafer, and film thickness measurement is carried out: the interface of the unintentionally doped gallium oxide film, the AlGaO epitaxial film and the substrate can be clearly seen by SEM by using the position of a test point on the surface of a Focused Ion Beam (FIB) epitaxial wafer as a section fault, so that the thickness of the homoepitaxial gallium oxide film can be accurately measured, and the result is shown in Table 1:
TABLE 1 homoepitaxial gallium oxide film thickness measurement results
As can be seen from the results of Table 1, compared with the comparative example, the unintended doped gallium oxide film and AlGaO epitaxial film prepared by the method of the invention are closer to the target thickness, and the thickness standard deviation of the unintended doped gallium oxide film and AlGaO epitaxial film prepared by the method of the invention is smaller, which indicates that the homoepitaxial gallium oxide film prepared by the method of the invention has higher thickness uniformity and better quality.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.
Claims (3)
1. The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate based on the molecular beam epitaxy equipment is characterized by comprising the following steps:
a molecular pump is started in advance to vacuumize the MBE growth chamber;
fixing an unintended doped gallium oxide substrate at the bottom end of a stainless steel tray, and enabling the growth surface of the unintended doped gallium oxide substrate to face downwards;
stopping a molecular pump, filling nitrogen into a rapid sample injection cavity, and then, placing the stainless steel tray fixed with the unintended doped gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of a Ga metal evaporation source and an Al metal doping source, and setting the rapid flow intensity of the Ga metal evaporation source and the Al metal doping source when the Ga metal evaporation source and the Al metal doping source reach the preset evaporation temperature;
starting a molecular pump, vacuumizing the rapid sample injection cavity, and when the vacuum degree of the rapid sample injection cavity is lower than 10 -8 At mbar, transferring the stainless steel tray fixed with the unintended doped gallium oxide substrate into the MBE growth chamber, and opening the laser to heat the stainless steel tray;
slowly opening an oxygen plasma source pipeline angle valve, and setting the oxygen flow to be 0.1-0.5sccm on a digital flowmeter;
after the laser heats the stainless steel tray to a preset film growth temperature, an oxygen source is started, oxygen plasma is lightened, the oxygen pressure is waited to be stable, a baffle of the Ga metal evaporation source is controlled to be set in an automatic mode, and the unintended homoepitaxial growth of the gallium oxide doped film is carried out;
monitoring that the unintended doped gallium oxide film is homoepitaxially grown to a first preset thickness, keeping the supply of an oxygen source and a Ga metal evaporation source, setting a baffle plate of an Al metal doping source to be in an automatic mode, continuously growing an AlGaO epitaxial film on the unintended doped gallium oxide film, and controlling the doping mole percentage of Al to be not more than 23%;
after the AlGaO epitaxial film grows to a second preset thickness, the baffle plates of the Ga metal evaporation source and the Al metal doping source are automatically closed, the oxygen source supply is kept, the cooling rate of the stainless steel tray is set to be 5-35 ℃/min, when the temperature of the stainless steel tray is lower than 200 ℃, the oxygen source is cut off, the laser is closed, and the preparation of the unintended doped gallium oxide film and the AlGaO epitaxial film on the high-resistance substrate is completed;
pre-starting molecular pump to MBE growthIn the step of evacuating the chamber, the MBE growth chamber is evacuated to a temperature of less than 2X 10 -9 mbar; the preset evaporation temperature of the Ga metal evaporation source and the Al metal doping source is 1000-1200 ℃, and the heating rate is 2-10 ℃/min; the rapid flow strength of the Ga metal evaporation source and the Al metal doping source is 1 multiplied by 10 -8 -9×10 -7 mbar; the laser heats the stainless steel tray to a preset film growth temperature, wherein the preset film growth temperature is 600-1000 ℃, and the heating rate is 5-15 ℃/min;
the molecular beam epitaxy equipment comprises an MBE growth chamber, a stainless steel tray arranged in the MBE growth chamber and a high-resistance gallium oxide substrate arranged at the bottom end of the stainless steel tray, wherein a laser is arranged below the stainless steel tray, and a laser spot emitted by the laser covers the whole bottom end of the stainless steel tray; the laser is provided with a beam expander; the laser emitted by the laser has a wavelength of 800-1200nm.
2. The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate based on the molecular beam epitaxy equipment according to claim 1, wherein the homoepitaxial growth speed of the unintended doped gallium oxide film is 10-100 nanometers/hour, and the first preset thickness is 100-500 nanometers.
3. The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate based on the molecular beam epitaxy equipment according to claim 1, wherein the growth speed of the AlGaO epitaxial film is 10-50 nanometers/hour, and the second preset thickness is 10-60nm.
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| JP2005019492A (en) * | 2003-06-24 | 2005-01-20 | Ishikawajima Harima Heavy Ind Co Ltd | Compound semiconductor growing device |
| CN1728349A (en) * | 2004-07-28 | 2006-02-01 | 中国科学院半导体研究所 | The manufacture method of aluminum-gallium-nitrogen/gallium nitride transistor with high electron mobility |
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