CN114908419B - Method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate and MOCVD equipment - Google Patents
Method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate and MOCVD equipment Download PDFInfo
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- CN114908419B CN114908419B CN202210465463.XA CN202210465463A CN114908419B CN 114908419 B CN114908419 B CN 114908419B CN 202210465463 A CN202210465463 A CN 202210465463A CN 114908419 B CN114908419 B CN 114908419B
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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 228
- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 228
- 239000000758 substrate Substances 0.000 title claims abstract description 109
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 title claims abstract 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 64
- 239000010439 graphite Substances 0.000 claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 claims abstract description 56
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 82
- 239000001301 oxygen Substances 0.000 claims description 82
- 229910052760 oxygen Inorganic materials 0.000 claims description 82
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 74
- 229910052733 gallium Inorganic materials 0.000 claims description 74
- 239000012159 carrier gas Substances 0.000 claims description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 230000001105 regulatory effect Effects 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000005520 cutting process Methods 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 238000012544 monitoring process Methods 0.000 claims description 14
- 230000001276 controlling effect Effects 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000005070 sampling Methods 0.000 claims description 7
- 229910000077 silane Inorganic materials 0.000 claims description 7
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical group CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 claims description 7
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 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 97
- 230000006698 induction Effects 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- YBBZWHIIYJKMKV-UHFFFAOYSA-N Barbatin Chemical compound CC1=C(O)C(C(=O)OC)=C(C)C=C1OC(=O)C1=C(C)C=C(OC)C(C)=C1O YBBZWHIIYJKMKV-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 2
- 229930190801 barbatin Natural products 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 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
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004857 zone melting 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
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/48—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation
- C23C16/481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation by radiant heating of the substrate
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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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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- C30B25/10—Heating of the reaction chamber or the substrate
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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 MOCVD equipment, wherein the method comprises an MOCVD reaction cavity, a graphite tray arranged in the MOCVD reaction cavity and the high-resistance gallium oxide substrate arranged on the graphite 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 graphite tray through the high-resistance gallium oxide substrate, so that the graphite tray in the MOCVD reaction cavity can be uniformly heated in a laser heating mode through the laser arranged above the graphite 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.
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 MOCVD equipment.
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 5 crystal structures, respectively in rhombohedral (alpha) and monoclinic system(beta), defective spinel (gamma), cube (delta) and orthorhombic crystal (epsilon). 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 。
Gallium oxide has the following advantages: (1) The forbidden bandwidth is 4.8-4.9 eV, and the breakdown field strength is as high as 8MV/cm. The Barbatin figure of merit is a low loss performance index in the semiconductor field, whereas the Barbatin figure of merit for gallium oxide is as high as 3400, approximately 10 times that for SiC, 4 times that for GaN. Therefore, when manufacturing the unipolar power device with the same withstand voltage, the on-resistance of the element is much lower than that of SiC and GaN, and the on-loss of the device is greatly reduced; (2) A large-sized and high-quality gallium oxide single crystal substrate material can be grown by a fusion method such as a zone-melting method (Fz), a czochralski method (Cz), or a guided-mode method (EFG), and a gallium oxide wafer can be obtained from a bulk single crystal. Compared with SiC and GaN growth technologies, the method is easier to obtain high-quality low-cost monocrystalline materials; (3) Among the epitaxial methods of gallium oxide, the Metal Oxide Chemical Vapor Deposition (MOCVD) method has the best comprehensive performance in terms of growth speed, film quality, in-situ detection, mass production and other convenience, and is most suitable for future industrialized mass production. Thus, an unintentionally doped gallium oxide buffer layer film and a weakly conductive gallium oxide film can be sequentially homoepitaxially grown on a high-resistance gallium oxide substrate using an MOCVD apparatus for preparing high-performance lateral metal-oxide semiconductor field effect transistor (MOSFET) devices.
Aiming at the technical characteristics of the existing MOCVD, in the process of preparing the gallium oxide homoepitaxial film by using MOCVD 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, there are two methods to achieve heating of gallium oxide substrates: (1) Transmitting heat to the graphite tray through a heating wire arranged below the graphite tray, so as to heat the gallium oxide substrate on the graphite tray; (2) The graphite tray inside the reaction chamber is heated by an induction coil arranged outside the reaction chamber, and heat is transferred to the gallium oxide substrate on the graphite tray. However, in the method (1), since there is always a certain spatial distribution of the arrangement of the heating wires, the heating of the graphite tray is uneven, and the substrate on the graphite tray is naturally also unevenly heated; in the method (2), as the radio frequency heating has a skin effect and the corners of the heated materials have a centralized heating effect, the heating of the graphite tray is uneven in the process of heating the graphite tray, the substrate is naturally heated unevenly, the thickness uniformity of the prepared epitaxial wafer is seriously affected, and even the epitaxial wafer 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 and an MOCVD apparatus for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate, which aims 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 MOCVD equipment for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises an MOCVD reaction cavity, a graphite tray arranged in the MOCVD reaction cavity and the high-resistance gallium oxide substrate arranged on the graphite tray, wherein a laser is arranged above the graphite tray, and a laser spot emitted by the laser covers the whole top of the graphite tray.
The MOCVD equipment for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate is characterized in that at least one laser is arranged above the graphite tray.
The MOCVD 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 MOCVD equipment for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises a laser, wherein 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 MOCVD equipment comprises the following steps:
placing the high-resistance gallium oxide substrate on a graphite tray, and closing the MOCVD reaction cavity;
starting a laser to raise the temperature of the high-resistance gallium oxide substrate to be 20-200 ℃ higher than the growth temperature of the homoepitaxial gallium oxide film, and performing heat treatment for 30-300 min;
adjusting the power of a laser to reduce the temperature of a high-resistance gallium oxide substrate to the growth temperature of an epitaxial film at 600-1100 ℃, sequentially introducing a gallium source and an oxygen source into the MOCVD reaction cavity, and growing an unintended doped gallium oxide buffer layer on the high-resistance gallium oxide substrate;
monitoring the growth of the unintended doped gallium oxide buffer layer to a first preset thickness, and sequentially cutting off the supply of an oxygen source and a gallium source;
sequentially introducing a gallium source, a doping source and an oxygen source into the MOCVD reaction cavity, and continuously growing a weak-conductivity gallium oxide film on the unintentional doped gallium oxide buffer layer;
and after monitoring that the weakly conductive gallium oxide film grows to a second preset thickness, cutting off the supply of an oxygen source, a doping source and a gallium source in sequence to finish the preparation of the homoepitaxial gallium oxide film.
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises the steps of introducing trimethyl gallium into a gallium source in the process of growing an unintended doped gallium oxide buffer layer on the high-resistance gallium oxide substrate, selecting argon as carrier gas, adjusting the temperature of the gallium source to be-10-40 ℃, the flow rate of the gallium source to be 10-200sccm, and the flow rate of the carrier gas to be 100-2000sccm; the oxygen source is oxygen, and the flow rate of the oxygen source is 200-2000sccm.
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises the steps of continuously growing a weak-conductivity gallium oxide film on the unintended doped gallium oxide buffer layer, wherein the introduced gallium source is triethyl gallium, argon is selected as carrier gas, the temperature of the gallium source is regulated to be 0-50 ℃, the flow rate of the gallium source is 20-500sccm, and the flow rate of the carrier gas is 200-5000sccm; the doping source is silane, the temperature of the doping source is regulated to be-5-25 ℃, and the flow is 1-10sccm; the oxygen source is oxygen, and the flow rate of the oxygen source is 200-2000sccm.
The method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate comprises the steps of wherein the doped carrier concentration of the weak-conductivity gallium oxide film is 1 multiplied by 10 16 /cm 3 -2×10 17 /cm 3 。
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises the steps of enabling the first predicted thickness to be 0.5-1.5 microns and enabling the second predicted thickness to be 0.1-1 microns.
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate comprises the following steps of:
and controlling the high-resistance gallium oxide substrate to cool to room temperature at a cooling rate of 20-200 ℃/h, sampling, and closing the laser.
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 MOCVD 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 graphite tray through the high-resistance gallium oxide substrate, so that the graphite tray in the MOCVD reaction cavity can be uniformly heated in a laser heating mode through the laser arranged above the graphite 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 the structure of MOCVD equipment 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 MOCVD equipment, and the invention is further described in detail below for making 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 film during the preparation of the gallium oxide homoepitaxial film using the MOCVD equipment. The heating mode of the gallium oxide substrate in the existing MOCVD 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 the above, the invention provides MOCVD equipment for preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate, which comprises an MOCVD reaction cavity 10, a graphite tray 20 arranged in the MOCVD reaction cavity 10 and a high-resistance gallium oxide substrate 30 arranged on the graphite tray 20, wherein a laser 40 is arranged above the graphite tray 20, and a laser spot emitted by the laser 40 covers the whole top of the graphite 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 2O3 single crystals and the annealing effects). That is, since the absorption of the infrared laser by the high-resistance gallium oxide substrate is extremely small, the laser directly irradiates the high-resistance gallium oxide substrate and can be directly transmitted to irradiate the graphite tray in the process of heating the high-resistance gallium oxide substrate by using the laser of the common infrared band. Therefore, the graphite tray in the MOCVD reaction cavity can be uniformly heated in a laser heating mode through the laser arranged above the graphite 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 a high-performance transverse MOSFET device.
In some embodiments, at least 1 laser is disposed above the graphite tray. As an example, 2 lasers can be arranged above the graphite tray; 3, 4, 5, 6, etc. may be provided. When 2 or more lasers are arranged, only the lasers emitted by the lasers need to be ensured to uniformly cover the top of the graphite 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 entire graphite 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 an MOCVD apparatus, as shown in fig. 3, comprising the steps of:
s10, placing a high-resistance gallium oxide substrate on a graphite tray, and closing an MOCVD reaction cavity;
s20, turning on a laser to raise the temperature of the high-resistance gallium oxide substrate to 20-200 ℃ higher than the growth temperature of the homoepitaxial gallium oxide film, and performing heat treatment for 30-300 min;
s30, adjusting the power of a laser to reduce the temperature of the high-resistance gallium oxide substrate to the epitaxial film growth temperature of 600-1100 ℃, sequentially introducing a gallium source and an oxygen source into the MOCVD reaction chamber, and growing an unintended doped gallium oxide buffer layer on the high-resistance gallium oxide substrate;
s40, monitoring the growth of the unintended doped gallium oxide buffer layer to a first preset thickness, and sequentially cutting off the supply of an oxygen source and a gallium source;
s50, sequentially introducing a gallium source, a doping source and an oxygen source into the MOCVD reaction chamber, and continuously growing a weak-conductivity gallium oxide film on the unintentional doped gallium oxide buffer layer;
and S60, monitoring the growth of the weak-conductivity gallium oxide film to a second preset thickness, and sequentially cutting off the supply of an oxygen source, a doping source and a gallium source to finish the preparation of the homoepitaxial gallium oxide film.
In the embodiment, the heating temperature of the graphite 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 flow rates of the gallium source and the oxygen source. In the process of preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate, the graphite tray is kept static, so that the disturbance of rotation to the growth process of the homoepitaxial gallium oxide film is reduced as much as possible, and the graphite tray is uniformly heated under the irradiation of laser, so that the uniform heating of the high-resistance gallium oxide substrate is realized. 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 graphite tray in the reaction cavity of the MOCVD 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 buffer layer and a weak-conductivity gallium oxide film are prepared and used for preparing a high-performance transverse MOSFET device.
In some embodiments, in the process of growing an unintended doped gallium oxide buffer layer on the high-resistance gallium oxide substrate, the introduced gallium source is trimethyl gallium, argon is selected as carrier gas, the temperature of the gallium source is regulated to be-10-40 ℃, the flow rate of the gallium source is 10-200sccm, and the flow rate of the carrier gas is 100-2000sccm; the oxygen source is oxygen, and the flow rate of the oxygen source is 200-2000sccm. In this example, the growth rate of the unintentionally doped gallium oxide buffer layer was controlled to be 0.5-5 μm/hr by adjusting the flow rates of the gallium source and the oxygen source.
In some embodiments, in the process of continuously growing the weak-conductivity gallium oxide film on the unintentionally doped gallium oxide buffer layer, the introduced gallium source is triethyl gallium, argon is selected as carrier gas, the temperature of the gallium source is regulated to be 0-50 ℃, the flow rate of the gallium source is 20-500sccm, and the flow rate of the carrier gas is 200-5000sccm; the doping source is silane, the temperature of the doping source is regulated to be-5-25 ℃, and the flow is 1-10sccm; the oxygen source is oxygen, and the flow rate of the oxygen source is 200-2000sccm. In this example, the growth rate of the weakly conductive gallium oxide film was controlled to 0.1-1 μm/hr by adjusting the flow rates of the gallium source, the doping source and the oxygen source.
In some embodiments, the doped carrier concentration of the weakly conductive gallium oxide film is 1×10 16 /cm 3 -2×10 17 /cm 3 。
In some embodiments, the first predicted thickness is 0.5-1.5 microns and the second predicted thickness is 0.1-1 microns.
In some embodiments, the method further comprises the step of, after cutting off the supply of the oxygen source, the doping source and the gallium source: and controlling the high-resistance gallium oxide substrate to cool to room temperature at a cooling rate of 20-200 ℃/h, sampling, and closing the laser to finish the preparation of the homoepitaxial gallium oxide buffer layer and the weak-conductivity gallium oxide film on the high-resistance gallium oxide substrate.
The invention is further illustrated by the following examples:
example 1
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate based on MOCVD equipment comprises an MOCVD reaction cavity, a graphite tray arranged in the MOCVD reaction cavity and the high-resistance gallium oxide substrate arranged on the graphite tray, wherein 1 laser is arranged above the graphite tray, and laser spots emitted by the lasers cover the whole top of the graphite tray; the method comprises the following steps:
placing a 4-inch Fe-doped high-resistance gallium oxide substrate on a graphite tray, and closing an MOCVD reaction cavity;
turning on a laser to raise the temperature of the high-resistance gallium oxide substrate to be 100 ℃ higher than the growth temperature of the homoepitaxial gallium oxide film, and performing heat treatment for 200 min;
adjusting the power of a laser to reduce the temperature of the high-resistance gallium oxide substrate to the growth temperature of an epitaxial film at 900 ℃, and preparing an unintentionally doped gallium oxide buffer layer;
selecting trimethyl gallium as a gallium source, selecting argon as carrier gas, adjusting the temperature of the gallium source to 20 ℃, the flow rate to 100sccm and the carrier gas flow rate to 1000sccm, and introducing the gallium source into a reaction cavity;
after 5 minutes, oxygen source is introduced into the reaction cavity, oxygen is selected as the oxygen source, and the flow of the oxygen is regulated to 1000sccm;
according to the thickness monitoring system, the growth speed and thickness of the epitaxial film are fed back in real time, and the flow rates of a gallium source and an oxygen source are flexibly regulated, so that the growth speed of the epitaxial film is controlled to be 2.5 microns/hour until the thickness of the buffer layer reaches 1 micron;
cutting off the supply of oxygen source and gallium source in turn, and preparing the weak conductive gallium oxide film;
selecting triethyl gallium as a gallium source, selecting argon as carrier gas, adjusting the temperature of the gallium source to 25 ℃, the flow rate to 250sccm and the carrier gas flow rate to 2500sccm, and introducing the gallium source into a reaction cavity;
selecting silane as doping source, regulating the temperature of the doping source to 15 deg.C and the flow rate to 5sccm, introducing the doping source into the reaction cavity, and controlling the concentration range of doped carriers to 1×10 17 /cm 3 ；
After 5 minutes, oxygen source is introduced into the reaction cavity, oxygen is selected as the oxygen source, and the flow of the oxygen is regulated to 1000sccm;
according to the thickness monitoring system, the growth speed and thickness of the epitaxial film are fed back in real time, and the flow rates of a gallium source, a doping source and an oxygen source are flexibly adjusted, so that the growth speed of the epitaxial film is controlled to be 0.5 micron/hour until the thickness of a gallium oxide drift layer reaches 0.5 micron;
and cutting off the supply of the oxygen source, the doping source and the gallium source in sequence, controlling the substrate to be cooled to room temperature at the cooling rate of 100 ℃ per hour, sampling, and closing the laser to finish the preparation of the homoepitaxial gallium oxide buffer layer film and the weak conductive gallium oxide film on the high-resistance gallium oxide substrate.
Example 2
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate based on MOCVD equipment comprises an MOCVD reaction cavity, a graphite tray arranged in the MOCVD reaction cavity and the high-resistance gallium oxide substrate arranged on the graphite tray, wherein 1 laser is arranged above the graphite tray, and laser spots emitted by the lasers cover the whole top of the graphite tray; the method comprises the following steps:
placing a 4-inch Fe-doped high-resistance gallium oxide substrate on a graphite tray, and closing an MOCVD reaction cavity;
turning on a laser to raise the temperature of the high-resistance gallium oxide substrate to 200 ℃ higher than the growth temperature of the homoepitaxial gallium oxide film, and performing heat treatment for 300 min;
adjusting the power of a laser to reduce the temperature of the high-resistance gallium oxide substrate to the growth temperature of an epitaxial film at 1100 ℃, and preparing an unintentionally doped gallium oxide buffer layer;
selecting trimethyl gallium as a gallium source, selecting argon as carrier gas, adjusting the temperature of the gallium source to 40 ℃, the flow rate to 200sccm and the carrier gas flow rate to 2000sccm, and introducing the gallium source into a reaction cavity;
after 8 minutes, oxygen source is introduced into the reaction cavity, oxygen is selected as the oxygen source, and the flow rate of the oxygen is regulated to 2000sccm;
according to the thickness monitoring system, the growth speed and thickness of the epitaxial film are fed back in real time, and the flow rates of a gallium source and an oxygen source are flexibly regulated, so that the growth speed of the epitaxial film is controlled to be 5 microns/hour until the thickness of the buffer layer reaches 1.5 microns;
cutting off the supply of oxygen source and gallium source in turn, and preparing high-resistance gallium oxide floating film;
selecting triethyl gallium as a gallium source, selecting argon as carrier gas, adjusting the temperature of the gallium source to 50 ℃, the flow rate to 500sccm and the carrier gas flow rate to 5000sccm, and introducing the gallium source into a reaction cavity;
selecting silane as doping source, regulating the temperature of the doping source to 25deg.C and the flow rate to 10 sccm), introducing the doping source into the reaction chamber, and dopingCarrier concentration range is controlled to 2×10 17 /cm 3 ；
After 8 minutes, oxygen source is introduced into the reaction cavity, oxygen is selected as the oxygen source, and the flow rate of the oxygen is regulated to 2000sccm;
according to the thickness monitoring system, the growth speed and thickness of the epitaxial film are fed back in real time, and the flow rates of a gallium source, a doping source and an oxygen source are flexibly adjusted, so that the growth speed of the epitaxial film is controlled to be 1 micron/hour until the thickness of a gallium oxide drift layer reaches 1 micron;
and cutting off the supply of the oxygen source, the doping source and the gallium source in sequence, controlling the substrate to be cooled to room temperature at the cooling rate of 200 ℃/hour, sampling, and closing the laser to finish the preparation of the homoepitaxial gallium oxide buffer layer film and the weak conductive gallium oxide film on the high-resistance gallium oxide substrate.
Example 3
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate based on MOCVD equipment comprises an MOCVD reaction cavity, a graphite tray arranged in the MOCVD reaction cavity and the high-resistance gallium oxide substrate arranged on the graphite tray, wherein 1 laser is arranged above the graphite tray, and laser spots emitted by the lasers cover the whole top of the graphite tray; the method comprises the following steps:
placing a 4-inch Fe-doped high-resistance gallium oxide substrate on a graphite tray, and closing an MOCVD reaction cavity;
turning on a laser to raise the temperature of the high-resistance gallium oxide substrate to 20 ℃ higher than the growth temperature of the homoepitaxial gallium oxide film, and performing heat treatment for 30 min;
adjusting the power of a laser to reduce the temperature of the high-resistance gallium oxide substrate to the growth temperature of an epitaxial film at 600 ℃, and preparing an unintentionally doped gallium oxide buffer layer;
selecting trimethyl gallium as a gallium source, selecting argon as carrier gas, adjusting the temperature of the gallium source to-10 ℃, the flow rate to 10 and the carrier gas flow rate to 100, and introducing the gallium source into a reaction cavity;
after 3 minutes, oxygen source is introduced into the reaction cavity, oxygen is selected as the oxygen source, and the flow of the oxygen is regulated to be 200sccm;
according to the thickness monitoring system, the growth speed and thickness of the epitaxial film are fed back in real time, and the flow rates of a gallium source and an oxygen source are flexibly regulated, so that the growth speed of the epitaxial film is controlled to be 1 micron/hour until the thickness of the buffer layer reaches 0.5 micron;
cutting off the supply of oxygen source and gallium source in turn, and preparing the weak conductive gallium oxide film;
selecting triethyl gallium as a gallium source, selecting argon as carrier gas, adjusting the temperature of the gallium source to 0 ℃, the flow of the carrier gas to 20sccm and the flow of the carrier gas to 200sccm, and introducing the gallium source into a reaction cavity;
selecting silane as doping source, regulating the temperature of the doping source to 5 deg.c and flow rate to 2sccm, introducing the doping source into the reaction cavity, and controlling the concentration range of doped carrier to 1×10 16 /cm 3 ；
After 3 minutes, oxygen source is introduced into the reaction cavity, oxygen is selected as the oxygen source, and the flow of the oxygen is regulated to be 500sccm;
according to the thickness monitoring system, the growth speed and thickness of the epitaxial film are fed back in real time, and the flow rates of a gallium source, a doping source and an oxygen source are flexibly adjusted, so that the growth speed of the epitaxial film is controlled to be 0.2 micron/hour until the thickness of a gallium oxide drift layer reaches 0.5 micron;
and cutting off the supply of the oxygen source, the doping source and the gallium source in sequence, controlling the substrate to be cooled to room temperature at the cooling rate of 50 ℃/hour, sampling, and closing the laser to finish the preparation of the homoepitaxial gallium oxide buffer layer film and the weak conductive gallium oxide film on the high-resistance gallium oxide substrate.
Comparative example 1
The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate based on MOCVD equipment comprises an MOCVD reaction cavity, a graphite tray arranged in the MOCVD reaction cavity and the high-resistance gallium oxide substrate arranged on the graphite tray, wherein an induction coil is arranged on the outer side of the MOCVD reaction cavity, and the graphite tray is heated through the induction coil so as to transfer heat to the high-resistance gallium oxide substrate on the graphite tray; the method comprises the following steps:
placing a 4-inch Fe-doped high-resistance gallium oxide substrate on a graphite tray, and closing an MOCVD reaction cavity;
switching on the induction coil power supply to raise the temperature of the high-resistance gallium oxide substrate to be 100 ℃ higher than the growth temperature of the homoepitaxial gallium oxide film, and performing heat treatment for 200 min;
adjusting the heating power of the induction coil to reduce the temperature of the high-resistance gallium oxide substrate to the epitaxial film growth temperature of 900 ℃ and preparing an unintended doped gallium oxide buffer layer;
selecting trimethyl gallium as a gallium source, selecting argon as carrier gas, adjusting the temperature of the gallium source to 20 ℃, the flow rate to 100sccm and the carrier gas flow rate to 1000sccm, and introducing the gallium source into a reaction cavity;
after 5 minutes, oxygen source is introduced into the reaction cavity, oxygen is selected as the oxygen source, and the flow of the oxygen is regulated to 1000sccm;
according to the thickness monitoring system, the growth speed and thickness of the epitaxial film are fed back in real time, and the flow rates of a gallium source and an oxygen source are flexibly regulated, so that the growth speed of the epitaxial film is controlled to be 2.5 microns/hour until the thickness of the buffer layer reaches 1 micron;
cutting off the supply of oxygen source and gallium source in turn, and preparing the weak conductive gallium oxide film;
selecting triethyl gallium as a gallium source, selecting argon as carrier gas, adjusting the temperature of the gallium source to 25 ℃, the flow rate to 250sccm and the carrier gas flow rate to 2500sccm, and introducing the gallium source into a reaction cavity;
selecting silane as doping source, regulating the temperature of the doping source to 15 deg.C and the flow rate to 5sccm, introducing the doping source into the reaction cavity, and controlling the concentration range of doped carriers to 1×10 17 /cm 3 ；
After 5 minutes, oxygen source is introduced into the reaction cavity, oxygen is selected as the oxygen source, and the flow of the oxygen is regulated to 1000sccm;
according to the thickness monitoring system, the growth speed and thickness of the epitaxial film are fed back in real time, and the flow rates of a gallium source, a doping source and an oxygen source are flexibly adjusted, so that the growth speed of the epitaxial film is controlled to be 0.5 micron/hour until the thickness of a gallium oxide drift layer reaches 0.5 micron;
and cutting off the supply of the oxygen source, the doping source and the gallium source in sequence, controlling the substrate to be cooled to room temperature at the cooling rate of 100 ℃ per hour, sampling, closing the power supply of the induction coil, and completing the preparation of the homoepitaxial gallium oxide buffer layer film and the weak conductive gallium oxide film on the high-resistance gallium oxide substrate.
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 buffer layer, the weak conductive gallium oxide film and the substrate can be clearly seen by using a Focused Ion Beam (FIB) epitaxial wafer surface test point position as a section fault, and further 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 buffer layer and the weak conductive gallium oxide 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 buffer layer and the weak conductive gallium oxide 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 (6)
1. The method for preparing the homoepitaxial gallium oxide film on the high-resistance gallium oxide substrate based on the MOCVD equipment is characterized in that the MOCVD equipment comprises an MOCVD reaction cavity and a graphite tray arranged in the MOCVD reaction cavity, a laser is arranged above the graphite tray, and a laser spot emitted by the laser covers the whole top of the graphite tray; the method comprises the steps of:
placing the high-resistance gallium oxide substrate on a graphite tray, and closing the MOCVD reaction cavity;
starting a laser to raise the temperature of the high-resistance gallium oxide substrate to be 20-200 ℃ higher than the growth temperature of the homoepitaxial gallium oxide film, and performing heat treatment for 30-300 min;
adjusting the power of a laser to reduce the temperature of a high-resistance gallium oxide substrate to the growth temperature of an epitaxial film at 600-1100 ℃, sequentially introducing a gallium source and an oxygen source into the MOCVD reaction cavity, and growing an unintended doped gallium oxide buffer layer on the high-resistance gallium oxide substrate;
monitoring the growth of the unintended doped gallium oxide buffer layer to a first preset thickness, and sequentially cutting off the supply of an oxygen source and a gallium source;
sequentially introducing a gallium source, a doping source and an oxygen source into the MOCVD reaction cavity, and continuously growing a weak-conductivity gallium oxide film on the unintentional doped gallium oxide buffer layer;
monitoring the growth of the weak-conductivity gallium oxide film to a second preset thickness, sequentially cutting off the supply of an oxygen source, a doping source and a gallium source, controlling the high-resistance gallium oxide substrate to cool to room temperature at a cooling rate of 20-200 ℃/hour, sampling, and closing a laser to finish the preparation of the homoepitaxial gallium oxide film; in the process of growing an unintended doped gallium oxide buffer layer on the high-resistance gallium oxide substrate, introducing trimethyl gallium serving as a gallium source, selecting argon as a carrier gas, adjusting the temperature of the gallium source to be-10-40 ℃, and adjusting the flow rate of the gallium source to be 10-200sccm and the flow rate of the carrier gas to be 100-2000sccm; the oxygen source is oxygen, and the flow rate of the oxygen source is 200-2000sccm;
in the process of continuously growing the weak-conductivity gallium oxide film on the unintended doped gallium oxide buffer layer, the introduced gallium source is triethyl gallium, argon is selected as carrier gas, the temperature of the gallium source is regulated to be 0-50 ℃, the flow rate of the gallium source is 20-500sccm, and the flow rate of the carrier gas is 200-5000sccm; the doping source is silane, the temperature of the doping source is regulated to be-5-25 ℃, and the flow is 1-10sccm; the oxygen source is oxygen, and the flow rate of the oxygen source is 200-2000sccm.
2. The method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate according to claim 1, wherein the doped carrier concentration of the weakly conductive gallium oxide film is 1×10 16 /cm 3 -2×10 17 /cm 3 。
3. The method of preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate according to claim 1, wherein the first predetermined thickness is 0.5 to 1.5 microns and the second predetermined thickness is 0.1 to 1 micron.
4. The method of preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate according to claim 1, wherein at least one laser is disposed above the graphite tray.
5. The method of preparing a homoepitaxial gallium oxide film on a high-resistance gallium oxide substrate according to claim 1, wherein a beam expander is provided on the laser.
6. The method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate according to claim 1, wherein the laser emits laser light with wavelength of 500-1500nm.
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| CN102051593A (en) * | 2010-11-29 | 2011-05-11 | 中山大学佛山研究院 | Method and device for epitaxially growing metal oxide transparent conductive film |
| CN103489967A (en) * | 2013-09-05 | 2014-01-01 | 大连理工大学 | Method for preparing gallium oxide epitaxial film and gallium oxide epitaxial film |
| CN107574479A (en) * | 2017-08-14 | 2018-01-12 | 南京大学 | A kind of multi-functional hydride vapor phase epitaxy growth system and application |
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| JP2005019492A (en) * | 2003-06-24 | 2005-01-20 | Ishikawajima Harima Heavy Ind Co Ltd | Compound semiconductor growing device |
| CN102051593A (en) * | 2010-11-29 | 2011-05-11 | 中山大学佛山研究院 | Method and device for epitaxially growing metal oxide transparent conductive film |
| CN103489967A (en) * | 2013-09-05 | 2014-01-01 | 大连理工大学 | Method for preparing gallium oxide epitaxial film and gallium oxide epitaxial film |
| CN107574479A (en) * | 2017-08-14 | 2018-01-12 | 南京大学 | A kind of multi-functional hydride vapor phase epitaxy growth system and application |
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