CN114808118A - Method for preparing homoepitaxial gallium oxide film on conductive gallium oxide substrate and molecular beam epitaxy equipment - Google Patents
Method for preparing homoepitaxial gallium oxide film on conductive gallium oxide substrate and molecular beam epitaxy equipment Download PDFInfo
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- CN114808118A CN114808118A CN202210466528.2A CN202210466528A CN114808118A CN 114808118 A CN114808118 A CN 114808118A CN 202210466528 A CN202210466528 A CN 202210466528A CN 114808118 A CN114808118 A CN 114808118A
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- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 247
- 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 246
- 239000000758 substrate Substances 0.000 title claims abstract description 167
- 238000001451 molecular beam epitaxy Methods 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 43
- 239000010935 stainless steel Substances 0.000 claims abstract description 43
- 239000010408 film Substances 0.000 claims description 78
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 43
- 239000001301 oxygen Substances 0.000 claims description 43
- 229910052760 oxygen Inorganic materials 0.000 claims description 43
- 238000001883 metal evaporation Methods 0.000 claims description 37
- 230000008020 evaporation Effects 0.000 claims description 21
- 238000001704 evaporation Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 21
- 239000010409 thin film Substances 0.000 claims description 18
- 238000002347 injection Methods 0.000 claims description 16
- 239000007924 injection Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 10
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000004907 flux Effects 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 238000007740 vapor deposition Methods 0.000 claims 1
- 238000004093 laser heating Methods 0.000 abstract description 3
- 235000012431 wafers Nutrition 0.000 description 10
- 238000001816 cooling Methods 0.000 description 7
- 238000001657 homoepitaxy Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- 230000005611 electricity Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 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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- 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 conductive gallium oxide substrate and molecular beam epitaxy equipment, wherein the molecular beam epitaxy equipment comprises an MEB growth chamber, a stainless steel tray arranged in the MEB growth chamber and the conductive gallium oxide substrate arranged at the bottom end of the stainless steel tray, and is characterized in that a laser is correspondingly arranged below the conductive gallium oxide substrate, the laser wavelength emitted by the laser is 1800-2200nm, and a laser spot emitted by the laser covers the whole bottom of the conductive gallium oxide substrate. The conductive gallium oxide substrate in the MEB growth chamber is directly heated by the laser through a laser heating method, so that the conductive gallium oxide substrate is uniformly heated, and the high-quality and uniform-thickness unintended doped gallium oxide homoepitaxial wafer 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 homoepitaxy gallium oxide film on a conductive gallium oxide substrate and molecular beam epitaxy equipment.
Technical Field
Gallium oxide (Ga) 2 O 3 ) As a novel third generation wide bandgap semiconductor, the semiconductor has the advantages of ultra-wide bandgap, high breakdown field strength and the like. The material is a transparent oxide semiconductor material, and has wide application prospect in the fields of power semiconductor devices, ultraviolet detectors, gas sensors and optoelectronic devices due to excellent physicochemical characteristics, good conductivity and luminescence property. Gallium oxide has a crystal structure of 5, which are rhombohedral (α), monoclinic (β), defect spinel (γ), cubic (δ) and orthorhombic (ε), respectively. beta-Ga 2 O 3 Because of its stability at high temperature, it has become a focus of research at home and abroad in recent years, and it is not particularly stated that the gallium oxides mentioned below are all referred to as β -Ga 2 O 3 。
In the gallium oxide epitaxial method, Molecular Beam Epitaxy (MBE) is one of the main means for growing high-purity and high-quality gallium oxide epitaxial films, and the concentration of unintentionally doped impurities can be effectively reduced and the accurate regulation and control growth of atomic scale can be realized by using ultrahigh vacuum and high-purity source materials. The gallium oxide film epitaxially grown by MBE has the advantages of good crystal quality, smooth surface and controllable electronic concentration, which are necessary conditions for obtaining high-performance gallium oxide-based power electronic devices and photoelectric conversion devices. Therefore, the high-quality gallium oxide unintentionally-doped homoepitaxial wafer can be prepared on the conductive gallium oxide substrate by using equipment of MBE; and then preparing a layer of P-type NiO on the gallium oxide unintentionally doped homoepitaxial wafer to further form a pn junction, so that the P-type NiO can be used for preparing a high-performance solar blind ultraviolet detector, and the urgent need of the high-response-speed solar blind ultraviolet detector in extreme occasions is met.
Aiming at the technical characteristics of the existing MBE, in the process of preparing the gallium oxide homoepitaxial thin film by using MBE equipment, a gallium oxide substrate needs to be maintained in a high-temperature state suitable for the growth of the gallium oxide thin film. In the prior art, the heating of the gallium oxide substrate is realized by heating the gallium oxide substrate through heat radiation by a heating wire arranged behind the substrate. Because the arrangement of the heating wires always has certain spatial distribution, the heating of the substrate is uneven, the quality and the thickness uniformity of the prepared epitaxial wafer are seriously influenced, and even the epitaxial layer is cracked.
Accordingly, there is a need for improvements and developments in the art.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention provides a method for preparing a homoepitaxial gallium oxide thin film on a conductive gallium oxide substrate and a molecular beam epitaxy apparatus, which aims to solve the problem of poor quality and thickness uniformity of gallium oxide epitaxial wafers prepared on the conductive gallium oxide substrate in the prior art.
The technical scheme of the invention is as follows:
a molecular beam epitaxy device for preparing a homoepitaxial gallium oxide film on a conductive gallium oxide substrate comprises an MEB growth chamber, a stainless steel tray arranged in the MEB growth chamber and the conductive gallium oxide substrate arranged at the bottom end of the stainless steel tray, wherein a laser is correspondingly arranged below the conductive gallium oxide substrate, the laser wavelength emitted by the laser is 1800-2200nm, and the laser spot emitted by the laser covers the whole bottom of the corresponding conductive gallium oxide substrate.
The molecular beam epitaxy equipment for preparing the homoepitaxy gallium oxide film on the conduction type gallium oxide substrate is characterized in that at least one conduction type gallium oxide substrate is arranged on the stainless steel tray, and a laser is correspondingly arranged below each conduction type gallium oxide substrate.
The molecular beam epitaxy equipment for preparing the homoepitaxy gallium oxide film on the conductive gallium oxide substrate is characterized in that a beam expander is arranged on the laser.
A method for preparing a homoepitaxial gallium oxide film on a conductive gallium oxide substrate based on molecular beam epitaxy equipment comprises the following steps:
a molecular pump is started in advance to carry out vacuum pumping treatment on the MBE growth chamber;
fixing a conductive gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the conductive gallium oxide substrate faces downwards;
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 conductive gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of the Ga metal evaporation source, and controlling the fast flow strength of the Ga metal evaporation source when the Ga metal evaporation source reaches the preset evaporation temperature;
starting the molecular pump to vacuumize the rapid sample introduction cavity, and when the vacuum degree of the rapid sample introduction cavity is lower than 10 - 8 When mbar exists, the stainless steel tray fixed with the conductive gallium oxide substrate is conveyed into the MBE growth chamber, and the laser is turned on to heat the conductive gallium oxide substrate;
slowly opening an angle valve of the oxygen plasma source pipeline, and setting the oxygen flow on the digital flowmeter to be 0.2-1 sccm;
when the conductive gallium oxide substrate is heated to a preset film growth temperature by the laser, starting an oxygen source, introducing ozone, waiting for the oxygen pressure to be stable, controlling a baffle of a Ga metal evaporation source to be set to be in an automatic mode, and performing homoepitaxial gallium oxide film growth;
when the growth thickness of the homoepitaxial gallium oxide film reaches 50-500 nanometers, the growth is finished, the baffle plate of the Ga metal evaporation source is automatically closed, and the oxygen source supply is kept; and when the temperature of the conductive gallium oxide substrate is lower than 200 ℃, cutting off the oxygen source, and turning off the laser to finish the preparation of the homoepitaxial gallium oxide film.
The method for preparing the homoepitaxial gallium oxide film on the conductive gallium oxide substrate comprises the step of vacuumizing an MBE growth chamber by starting a molecular pump in advance, wherein the MBE growth chamber is vacuumized to be lower than 2 x 10 -9 mbar。
The method for preparing the homoepitaxial gallium oxide film on the conductive gallium oxide substrate comprises the steps of setting the evaporation temperature of the Ga metal evaporation source to be 1000-1200 ℃ in advance, and setting the heating rate to be 2-10 ℃/min.
The method for preparing homoepitaxial gallium oxide film on the conductive gallium oxide substrate comprises the steps of preparing a substrate, and preparing a substrate by using a conductive gallium oxide substrate, wherein the flow velocity intensity of the Ga metal evaporation source is 1 x 10 -8 -9×10 -7 mbar。
The method for preparing the homoepitaxial gallium oxide film on the conductive gallium oxide substrate comprises the step of heating the conductive gallium oxide substrate to the 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 conductive gallium oxide substrate is characterized in that the growth speed of the homoepitaxial gallium oxide film is 10-100 nanometers per hour.
The method for preparing the homoepitaxy gallium oxide film on the conductive gallium oxide substrate comprises the steps of conveying the prepared homoepitaxy gallium oxide film from an MBE growth chamber to a rapid sample introduction cavity after the homoepitaxy gallium oxide film is prepared, and sampling at normal pressure after vacuum breaking.
Has the advantages that: the invention provides a method for preparing a homoepitaxy gallium oxide film on a conductive gallium oxide substrate and molecular beam epitaxy equipment, wherein lasers are correspondingly arranged below the conductive gallium oxide substrate, the laser wavelength emitted by the lasers is 1800-2200nm, and laser spots emitted by the lasers cover the whole bottom of the corresponding conductive gallium oxide substrate. In the invention, the absorptivity of the conductive gallium oxide substrate to laser with the wavelength of 1800-2200nm is as high as about 90%, so that the conductive gallium oxide substrate in the MEB growth chamber can be directly heated by the laser in a laser heating method, the conductive gallium oxide substrate is uniformly heated, and the unintentional gallium oxide doped homoepitaxial wafer with high quality and uniform thickness is prepared.
Drawings
FIG. 1 is a schematic structural diagram of a molecular beam epitaxy apparatus for preparing a homoepitaxial gallium oxide film on a conductive gallium oxide substrate according to the present invention.
Fig. 2 is a graph showing transmittance of a Sn-doped (conductive type) gallium oxide substrate.
FIG. 3 is a flow chart of a method for fabricating homoepitaxial gallium oxide films on a conductive gallium oxide substrate.
Detailed Description
The invention provides a method for preparing a homoepitaxial gallium oxide film on a conductive gallium oxide substrate and molecular beam epitaxy equipment, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Because the gallium oxide substrate needs to be maintained in a high-temperature state suitable for the growth of the gallium oxide film in the process of preparing the gallium oxide homoepitaxial film by using the molecular beam epitaxy equipment. The heating mode of the gallium oxide substrate in the existing molecular beam epitaxy equipment can cause the substrate to be heated unevenly, so that the quality and the thickness uniformity of an epitaxial wafer are seriously influenced, and even the epitaxial wafer is cracked.
Based on this, the invention provides a molecular beam epitaxy apparatus for preparing homoepitaxial gallium oxide thin film on a conductive gallium oxide substrate, as shown in fig. 1, which includes an MEB growth chamber 10, a stainless steel tray 20 disposed in the MEB growth chamber 10, and a conductive gallium oxide substrate 30 disposed at the bottom end of the stainless steel tray 20, wherein a laser 40 is correspondingly disposed below the conductive gallium oxide substrate 30, the laser wavelength emitted by the laser 40 is 1800-2200nm, and the laser spot emitted by the laser 40 covers the entire bottom of the corresponding conductive gallium oxide substrate 30.
Specifically, the conductivity type gallium oxide substrate reported in the literature has a low transmittance in the infrared band mainly due to the strong plasma reflection of electrons, see FIG. 2 (data from laboratory measurements, equipment information: Lambda 1050+ ultraviolet/visible/near infrared spectrophotometer), and SCI paper: the explanation of plasma reflection of electrons in Structural and electronic engineering of Fe-doped β -Ga2O3 single crystals and the analytical effects. In the process of heating the conductive gallium oxide substrate by using common laser in an infrared band, particularly laser in a 2-micron band, the substrate absorbs infrared laser greatly, the absorption rate reaches about 90%, the heat of the laser can be directly absorbed by the substrate, and the conductive gallium oxide substrate in the MEB growth chamber can be uniformly heated only by directly irradiating the conductive gallium oxide substrate by using a laser with uniform energy distribution.
According to the molecular beam epitaxy apparatus for preparing the homoepitaxial gallium oxide thin film on the conductive gallium oxide substrate provided by the embodiment, the laser spot emitted by the laser 40 covers the whole bottom of the conductive gallium oxide substrate 30, so that the conductive gallium oxide substrate 30 in the MEB growth chamber can be uniformly heated in a laser heating manner, and the homoepitaxial gallium oxide thin film with high quality and uniform thickness can be prepared.
In some embodiments, at least one conductive gallium oxide substrate is disposed on the stainless steel tray, and a laser is disposed below each conductive gallium oxide substrate. By way of example, as shown in fig. 1, two conductive gallium oxide substrates are disposed at the bottom end of the stainless steel tray, and a laser is disposed directly below each conductive gallium oxide substrate. Of course, the bottom end of the stainless steel tray can also be provided with 3 or more conductive gallium oxide substrates, and correspondingly, a laser is arranged right below each conductive gallium oxide substrate. The laser spot emitted by each laser can cover the whole bottom of the corresponding conductive gallium oxide substrate.
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 entire bottom of the corresponding conductive gallium oxide substrate.
In some embodiments, there is also provided a method of preparing a homoepitaxial gallium oxide thin film on a conductive gallium oxide substrate based on a molecular beam epitaxy apparatus, as shown in fig. 3, which includes the steps of:
s10, pre-starting a molecular pump to vacuumize the MBE growth chamber;
s20, fixing the conductive gallium oxide substrate at the bottom end of the stainless steel tray, wherein the growth surface of the conductive gallium oxide substrate faces downwards;
s30, stopping the molecular pump, filling nitrogen into the rapid sample injection cavity for vacuum breaking, and then placing the stainless steel tray fixed with the conductive gallium oxide substrate into the rapid sample injection cavity;
s40, setting the evaporation temperature of the Ga metal evaporation source, and controlling the fast flow intensity of the Ga metal evaporation source when the Ga metal evaporation source reaches the preset evaporation temperature;
s50, starting a molecular pump, and vacuumizing the rapid sample introduction cavity when the vacuum degree of the rapid sample introduction cavity is lower than 10 -8 When mbar exists, the stainless steel tray fixed with the conductive gallium oxide substrate is conveyed into the MBE growth chamber, and the laser is turned on to heat the conductive gallium oxide substrate;
s60, slowly opening an angle valve of the oxygen plasma source pipeline, and setting the oxygen flow on the digital flowmeter to be 0.2-1 sccm;
s70, after the conductive gallium oxide substrate is heated to a preset film growth temperature by the laser, starting an oxygen source, introducing ozone, waiting for the oxygen pressure to be stable, setting the baffle control of the Ga metal evaporation source to be an automatic mode, and carrying out homoepitaxial gallium oxide film growth;
s80, when the growth thickness of the homoepitaxial gallium oxide film reaches 50-500 nanometers, the growth is finished, the baffle of the Ga metal evaporation source is automatically closed, and the oxygen source supply is kept; and when the temperature of the conductive gallium oxide substrate is lower than 200 ℃, cutting off the oxygen source, and turning off the laser to finish the preparation of the homoepitaxial gallium oxide film.
In this embodiment, the heating temperature of the conductive gallium oxide substrate can be adjusted by controlling the power of the laser; the growth speed of the epitaxial gallium oxide film can be controlled by adjusting the fast flow intensity of the Ga metal evaporation source and the flow of the oxygen source. In the process of preparing the homoepitaxial gallium oxide film on the conductive gallium oxide substrate, the conductive gallium oxide substrate is uniformly heated under the irradiation of laser. Meanwhile, the temperature of the conductive gallium oxide substrate is measured in real time through the temperature sensor and fed back to the laser, and then the output power of the laser is adjusted, so that the temperature of the conductive gallium oxide substrate is maintained in a temperature range suitable for the growth of the epitaxial gallium oxide film.
In some embodiments, the step of pre-priming the molecular pump to evacuate the MBE growth chamber comprises evacuating the MBE growth chamber to less than 2 × 10% -9 mbar。
In some embodiments, the predetermined evaporation temperature of the Ga metal evaporation source is 1000-.
In some embodiments, the rapid flow intensity of the Ga metal evaporation source is 1 × 10 -8 -9×10 -7 mbar, but not limited thereto.
In some embodiments, the step of heating the conductive gallium oxide substrate to a predetermined film growth temperature by the laser includes, but is not limited to, a predetermined film growth temperature of 600-1000 ℃ and a temperature increase rate of 5-15 ℃/min.
In some embodiments, the growth rate of the homoepitaxial gallium oxide thin film is 10-100 nm/hr, but is not limited thereto.
In some embodiments, after the preparation of the homoepitaxial gallium oxide film is completed, the prepared homoepitaxial gallium oxide film is transferred from the MBE growth chamber to the rapid sample injection cavity, and the sample is taken at normal pressure after vacuum breaking.
The invention is further illustrated by the following specific examples:
example 1
A method for preparing a homoepitaxial gallium oxide film on a conductive gallium oxide substrate based on a molecular beam epitaxy device, wherein the molecular beam epitaxy device comprises an MEB growth chamber, a stainless steel tray arranged in the MEB growth chamber, and two conductive gallium oxide substrates arranged at the bottom end of the stainless steel tray, 1 laser is correspondingly arranged below each conductive gallium oxide substrate, the laser wavelength emitted by each laser is 2000nm, and the laser spot emitted by each laser covers the whole bottom of the corresponding conductive gallium oxide substrate; the method comprises the following steps:
confirming MBE deviceThe water, electricity and gas supply is normal, a molecular pump is started in advance to vacuumize the MBE growth chamber until the vacuum degree is lower than 2 multiplied by 10 -9 mbar；
Fixing a 2-inch Sn-doped conductive gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the conductive gallium oxide substrate faces downwards;
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 conductive gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of a Ga metal evaporation source to be 1100 ℃, and increasing and reducing the temperature at the speed of 6 ℃/min; when the Ga metal evaporation source reaches the preset evaporation temperature, the beam current gauge is used for measuring the beam current intensity, and the temperature of the evaporation source is adjusted according to the stabilized reading of the beam current gauge so as to maintain the beam current intensity at 5 multiplied by 10 -7 mbar；
Starting the molecular pump to vacuumize the rapid sample introduction cavity, and when the vacuum degree of the rapid sample introduction cavity is lower than 10 - 8 When mbar occurs, the stainless steel tray fixed with the conductive gallium oxide substrate is conveyed into the MBE growth chamber, the laser is turned on to heat the conductive gallium oxide substrate to 800 ℃, and the temperature rise rate is set to be 10 ℃/min; meanwhile, the substrate temperature is measured in real time through a temperature sensor and fed back to the laser, and then the laser output power is adjusted, so that the substrate temperature is maintained in a temperature range suitable for epitaxial growth;
slowly opening an angle valve of the oxygen plasma source pipeline, and setting the oxygen flow on the digital flowmeter to be 0.5 sccm;
when the conductive gallium oxide substrate is heated to the preset film growth temperature of 800 ℃ by the laser, starting an oxygen source, introducing ozone, waiting for the oxygen pressure to be stable, controlling a baffle of a Ga metal evaporation source to be in an automatic mode, and controlling the growth speed to be 60 nanometers/hour to perform homoepitaxial gallium oxide film growth;
when the growth thickness of the homoepitaxial gallium oxide film reaches 300 nanometers, the growth is finished, the baffle of the Ga metal evaporation source is automatically closed, the supply of an oxygen source is kept, and the cooling rate of the conductive gallium oxide substrate is set to be 20 ℃/min; and when the temperature of the conductive gallium oxide substrate is lower than 200 ℃, cutting off the oxygen source, and turning off the laser to finish the preparation of the homoepitaxial gallium oxide film.
Example 2
A method for preparing a homoepitaxial gallium oxide film on a gallium oxide substrate based on a molecular beam epitaxy device, wherein the molecular beam epitaxy device comprises an MEB growth chamber, a stainless steel tray arranged in the MEB growth chamber, and two gallium oxide substrates arranged at the bottom end of the stainless steel tray, 1 laser is correspondingly arranged below each gallium oxide substrate, the laser wavelength emitted by each laser is 1900nm, and the laser spot emitted by each laser covers the whole bottom of the corresponding gallium oxide substrate; the method comprises the following steps:
confirming that water, electricity and gas supply of the MBE equipment is normal, and starting a molecular pump in advance to vacuumize the MBE growth chamber until the vacuum degree is lower than 2 multiplied by 10 -9 mbar；
Fixing a 2-inch Sn-doped conductive gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the conductive gallium oxide substrate faces downwards;
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 conductive gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of a Ga metal evaporation source at 1200 ℃, and the heating and cooling rates are 2 ℃/min; when the Ga metal evaporation source reaches the preset evaporation temperature, the beam current gauge is used for measuring the beam current intensity, and the temperature of the evaporation source is adjusted according to the stabilized reading of the beam current gauge so as to maintain the beam current intensity at 2 multiplied by 10 -7 mbar；
Starting the molecular pump to vacuumize the rapid sample introduction cavity, and when the vacuum degree of the rapid sample introduction cavity is lower than 10 - 8 When mbar exists, the stainless steel tray fixed with the conductive gallium oxide substrate is conveyed into the MBE growth chamber, the laser is turned on to heat the conductive gallium oxide substrate to 700 ℃, and the temperature rise rate is set to be 6 ℃/min; meanwhile, the temperature of the substrate is measured in real time through a temperature sensor and fed back to the laser, and further the temperature is measuredAdjusting the laser output power to maintain the substrate temperature in a temperature range suitable for epitaxial growth;
slowly opening an angle valve of the oxygen plasma source pipeline, and setting the oxygen flow on the digital flowmeter to be 0.3 sccm;
when the conductive gallium oxide substrate is heated to the preset film growth temperature of 700 ℃ by the laser, starting an oxygen source, introducing ozone, waiting for the oxygen pressure to be stable, controlling a baffle of a Ga metal evaporation source to be in an automatic mode, and controlling the growth speed to be 20 nanometers per hour to perform homoepitaxial gallium oxide film growth;
when the growth thickness of the homoepitaxial gallium oxide film reaches 300 nanometers, the growth is finished, the baffle plate of the Ga metal evaporation source is automatically closed, the oxygen source supply is kept, and the cooling rate of the conductive gallium oxide substrate is set to be 10 ℃/min; and when the temperature of the conductive gallium oxide substrate is lower than 200 ℃, cutting off the oxygen source, and turning off the laser to finish the preparation of the homoepitaxial gallium oxide film.
Example 3
A method for preparing a homoepitaxial gallium oxide film on a conductive gallium oxide substrate based on a molecular beam epitaxy device, wherein the molecular beam epitaxy device comprises an MEB growth chamber, a stainless steel tray arranged in the MEB growth chamber, and two conductive gallium oxide substrates arranged at the bottom end of the stainless steel tray, 1 laser is correspondingly arranged below each conductive gallium oxide substrate, the laser wavelength emitted by each laser is 2200nm, and the laser spot emitted by each laser covers the whole bottom of the corresponding conductive gallium oxide substrate; the method comprises the following steps:
confirming that water, electricity and gas supply of the MBE equipment is normal, and starting a molecular pump in advance to vacuumize the MBE growth chamber until the vacuum degree is lower than 2 multiplied by 10 -9 mbar；
Fixing a 2-inch Sn-doped conductive gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the conductive gallium oxide substrate faces downwards;
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 conductive gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of a Ga metal evaporation source at 1200 ℃, and the heating and cooling rate at 8 ℃/min; when the Ga metal evaporation source reaches the preset evaporation temperature, the beam current gauge is used for measuring the beam current intensity, and the temperature of the evaporation source is adjusted according to the stabilized reading of the beam current gauge so as to maintain the beam current intensity at 8 multiplied by 10 -7 mbar；
Starting the molecular pump to vacuumize the rapid sample introduction cavity, and when the vacuum degree of the rapid sample introduction cavity is lower than 10 - 8 When mbar exists, the stainless steel tray fixed with the conductive gallium oxide substrate is conveyed into the MBE growth chamber, the laser is turned on to heat the conductive gallium oxide substrate to 900 ℃, and the temperature rise rate is set to be 15 ℃/min; meanwhile, the substrate temperature is measured in real time through a temperature sensor and fed back to the laser, and then the laser output power is adjusted, so that the substrate temperature is maintained in a temperature range suitable for epitaxial growth;
slowly opening an angle valve of the oxygen plasma source pipeline, and setting the oxygen flow on the digital flowmeter to be 0.8 sccm;
when the conductive gallium oxide substrate is heated to the preset film growth temperature of 900 ℃ by the laser, starting an oxygen source, introducing ozone, waiting for the oxygen pressure to be stable, controlling a baffle of a Ga metal evaporation source to be in an automatic mode, and controlling the growth speed to be 90 nm/h to perform homoepitaxial gallium oxide film growth;
when the growth thickness of the homoepitaxial gallium oxide film reaches 300 nanometers, the growth is finished, the baffle plate of the Ga metal evaporation source is automatically closed, the oxygen source supply is kept, and the cooling rate of the conductive gallium oxide substrate is set to be 30 ℃/min; and when the temperature of the conductive gallium oxide substrate is lower than 200 ℃, cutting off the oxygen source, and turning off the laser to finish the preparation of the homoepitaxial gallium oxide film.
Comparative example 1
A method for preparing a homoepitaxial gallium oxide thin film on a conductive gallium oxide substrate based on a molecular beam epitaxy apparatus comprising an MEB growth chamber, a stainless steel tray disposed within the MEB growth chamber, and a conductive gallium oxide substrate disposed on the stainless steel tray, wherein a heating wire is disposed above the stainless steel tray; the method comprises the following steps:
confirming that water, electricity and gas supply of the MBE equipment is normal, and pre-starting a molecular pump to vacuumize the MBE growth chamber until the vacuum degree is lower than 2 multiplied by 10 -9 mbar；
Fixing a 2-inch Sn-doped conductive gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the conductive gallium oxide substrate faces downwards;
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 conductive gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of a Ga metal evaporation source to be 1100 ℃, and the heating and cooling rates to be 6 ℃/min; when the Ga metal evaporation source reaches the preset evaporation temperature, the beam current gauge is used for measuring the beam current intensity, and the temperature of the evaporation source is adjusted according to the stabilized reading of the beam current gauge so as to maintain the beam current intensity at 5 multiplied by 10 -7 mbar；
Starting the molecular pump to vacuumize the rapid sample introduction cavity, and when the vacuum degree of the rapid sample introduction cavity is lower than 10 - 8 When mbar occurs, the stainless steel tray fixed with the conductive gallium oxide substrate is conveyed into the MBE growth chamber, the power supply of the heating wire is turned on to heat the conductive gallium oxide substrate to 800 ℃, and the heating rate is set to be 10 ℃/min;
slowly opening an angle valve of the oxygen plasma source pipeline, and setting the oxygen flow on the digital flowmeter to be 0.5 sccm;
when the conductive gallium oxide substrate is heated to the preset film growth temperature of 800 ℃ by the heating wire, starting an oxygen source, introducing ozone, waiting for the oxygen pressure to be stable, controlling a baffle of a Ga metal evaporation source to be in an automatic mode, and controlling the growth speed to be 60 nanometers/hour to perform homoepitaxial gallium oxide film growth;
when the growth thickness of the homoepitaxial gallium oxide film reaches 300 nanometers, the growth is finished, the baffle plate of the Ga metal evaporation source is automatically closed, the oxygen source supply is kept, and the cooling rate of the conductive gallium oxide substrate is set to be 5-35 ℃/min; and when the temperature of the conductive gallium oxide substrate is lower than 200 ℃, cutting off the oxygen source, and turning off the power supply of the heating wire to finish the preparation of the homoepitaxial gallium oxide film.
Example 4
The thickness and thickness standard deviation of homoepitaxial gallium oxide thin films prepared in examples 1 to 3 and comparative example 1 were measured
After the preparation of the homoepitaxial gallium oxide film on the wafer is finished, selecting 32 points (8 points are distributed in four diameter directions at equal intervals, the four directions are at equal intervals of 45 degrees and do not contain the center of a circle) in a shape of Chinese character Mi on the wafer to measure the film thickness: the test point position on the surface of the epitaxial wafer of the Focused Ion Beam (FIB) is used as a cross section fault, the interface of the epitaxial layer and the substrate can be clearly seen by SEM, and the thickness of the homoepitaxial gallium oxide film can be accurately measured, and the result is shown in table 1:
TABLE 1 Homeotropic epitaxial gallium oxide film thickness measurement results
As can be seen from the results in Table 1, compared with the comparative example, the thickness of the homoepitaxial gallium oxide film prepared by the method of the invention is closer to the target thickness, and the standard deviation of the thickness of the homoepitaxial gallium oxide film prepared by the method of the invention is smaller, which shows that the homoepitaxial gallium oxide film prepared by the method of the invention has higher thickness uniformity and better quality.
It will be understood that the invention is not limited to the examples described above, but that modifications and variations will occur to those skilled in the art in light of the above teachings, and that all such modifications and variations are considered to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A molecular beam epitaxy device for preparing a homoepitaxial gallium oxide film on a conductive gallium oxide substrate comprises an MEB growth chamber, a stainless steel tray arranged in the MEB growth chamber and the conductive gallium oxide substrate arranged at the bottom end of the stainless steel tray, and is characterized in that a laser is correspondingly arranged below the conductive gallium oxide substrate, the laser wavelength emitted by the laser is 1800-2200nm, and the laser spot emitted by the laser covers the whole bottom of the corresponding conductive gallium oxide substrate.
2. The molecular beam epitaxy apparatus for preparing a homoepitaxial gallium oxide thin film on a gallium oxide substrate of a conductivity type according to claim 1, wherein at least one gallium oxide substrate of a conductivity type is disposed on the stainless steel tray, and a laser is disposed under each of the gallium oxide substrates of a conductivity type.
3. The molecular beam epitaxy apparatus for producing a homoepitaxial gallium oxide thin film on a conductive gallium oxide substrate according to claim 1, wherein a beam expander is provided on the laser.
4. A method for producing a homoepitaxial gallium oxide thin film on a conductive gallium oxide substrate based on the molecular beam epitaxy apparatus as claimed in any one of claims 1 to 3, comprising the steps of:
a molecular pump is started in advance to carry out vacuum pumping treatment on the MBE growth chamber;
fixing a conductive gallium oxide substrate at the bottom end of a stainless steel tray, wherein the growth surface of the conductive gallium oxide substrate faces downwards;
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 conductive gallium oxide substrate into the rapid sample injection cavity;
setting the evaporation temperature of the Ga metal evaporation source, and controlling the fast flow strength of the Ga metal evaporation source when the Ga metal evaporation source reaches the preset evaporation temperature;
starting the molecular pump to vacuumize the rapid sample introduction cavity, and when the vacuum degree of the rapid sample introduction cavity is lower than 10 -8 When mbar exists, the stainless steel tray fixed with the conductive gallium oxide substrate is conveyed into the MBE growth chamber, and the laser is turned on to heat the conductive gallium oxide substrate;
slowly opening an angle valve of the oxygen plasma source pipeline, and setting the oxygen flow on the digital flowmeter to be 0.2-1 sccm;
when the conductive gallium oxide substrate is heated to a preset film growth temperature by the laser, starting an oxygen source, introducing ozone, waiting for the oxygen pressure to be stable, controlling a baffle of a Ga metal evaporation source to be set to be in an automatic mode, and performing homoepitaxial gallium oxide film growth;
when the growth thickness of the homoepitaxial gallium oxide film reaches 50-500 nanometers, the growth is finished, the baffle plate of the Ga metal evaporation source is automatically closed, and the oxygen source supply is kept; and when the temperature of the conductive gallium oxide substrate is lower than 200 ℃, cutting off the oxygen source, and turning off the laser to finish the preparation of the homoepitaxial gallium oxide film.
5. The method for preparing homoepitaxial gallium oxide thin film on conductive gallium oxide substrate according to claim 4, wherein in the step of evacuating the MBE growth chamber by pre-starting the molecular pump, the MBE growth chamber is evacuated to less than 2 x 10 -9 mbar。
6. The method for preparing homoepitaxial gallium oxide thin film on conductive gallium oxide substrate according to claim 4, wherein the evaporation temperature of the Ga metal evaporation source is set to 1000-1200 ℃ in advance, and the temperature rise rate is 2-10 ℃/min.
7. The method for producing a homoepitaxial gallium oxide thin film on a conductive gallium oxide substrate according to claim 4, wherein the vapor deposition source of Ga metal has a flux intensity of 1 x 10 -8 -9×10 -7 mbar。
8. The method for preparing a homoepitaxial gallium oxide film on a conductive gallium oxide substrate according to claim 4, wherein the step of heating the conductive gallium oxide substrate to a predetermined film growth temperature by the laser comprises a predetermined film growth temperature of 600-1000 ℃ and a temperature rise rate of 5-15 ℃/min.
9. The method for producing a homoepitaxial gallium oxide thin film on a conductive gallium oxide substrate according to claim 4, wherein the growth rate of the homoepitaxial gallium oxide thin film is 10 to 100 nm/hr.
10. The method for preparing the homoepitaxial gallium oxide film on the conductive gallium oxide substrate according to claim 4, wherein after the homoepitaxial gallium oxide film is prepared, the prepared homoepitaxial gallium oxide film is transferred from the MBE growth chamber to the rapid sample injection cavity, and the sample is taken at normal pressure after the vacuum is broken.
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| JP2005019492A (en) * | 2003-06-24 | 2005-01-20 | Ishikawajima Harima Heavy Ind Co Ltd | Compound semiconductor growing device |
| JP2013056802A (en) * | 2011-09-08 | 2013-03-28 | Tamura Seisakusho Co Ltd | METHOD FOR PRODUCING β-Ga2O3 SINGLE CRYSTAL FILM AND LAMINATED CRYSTAL STRUCTURE |
| WO2013080972A1 (en) * | 2011-11-29 | 2013-06-06 | 株式会社タムラ製作所 | Method for producing ga2o3 crystal film |
| KR20200103578A (en) * | 2020-08-13 | 2020-09-02 | 한국세라믹기술원 | Manufacturing method of gallium oxide thin film for power semiconductor using dopant activation technoloty |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005019492A (en) * | 2003-06-24 | 2005-01-20 | Ishikawajima Harima Heavy Ind Co Ltd | Compound semiconductor growing device |
| JP2013056802A (en) * | 2011-09-08 | 2013-03-28 | Tamura Seisakusho Co Ltd | METHOD FOR PRODUCING β-Ga2O3 SINGLE CRYSTAL FILM AND LAMINATED CRYSTAL STRUCTURE |
| WO2013080972A1 (en) * | 2011-11-29 | 2013-06-06 | 株式会社タムラ製作所 | Method for producing ga2o3 crystal film |
| KR20200103578A (en) * | 2020-08-13 | 2020-09-02 | 한국세라믹기술원 | Manufacturing method of gallium oxide thin film for power semiconductor using dopant activation technoloty |
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| 曲敬信等主编: "表面工程手册", 化学工业出版社, pages: 280 * |
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