CN110616456B - Preparation method of high-quality kappa-phase gallium oxide epitaxial film - Google Patents

Preparation method of high-quality kappa-phase gallium oxide epitaxial film Download PDF

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CN110616456B
CN110616456B CN201911009760.8A CN201911009760A CN110616456B CN 110616456 B CN110616456 B CN 110616456B CN 201911009760 A CN201911009760 A CN 201911009760A CN 110616456 B CN110616456 B CN 110616456B
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temperature
gas
kappa
carrier gas
temperature zone
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CN110616456A (en
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叶建东
龚义清
郝景刚
陈选虎
任芳芳
顾书林
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Nanjing Research Institute Of Nanjing University
Nanjing University
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Nanjing Research Institute Of Nanjing University
Nanjing University
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/16—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • 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
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides

Abstract

Method for growing kappa-Ga by adopting halide vapor phase epitaxy2O3The film forming process includes the reaction between high purity metal Ga and HCl in mixed carrier gas in the first temperature area to produce gaseous GaCl and GaCl3Then under the push of carrier gas, the reaction product in the first temperature area reaction area enters the second temperature area growth area and mixes with the O of carrier gas2Reaction, growth of kappa-Ga on substrate2O3A film; the first temperature zone adopts higher temperature to make metal Ga source and gaseous HCl react, the temperature used in the first temperature zone is 800-1050 ℃, and the second temperature zone adopts lower temperature to make the product and O transported from the first temperature zone2And reacting, wherein the temperature of the second temperature zone is 500-650 ℃. The method has the advantages of high growth speed, low cost and low toxicity of the required reactants, and can be used for preparing the kappa-Ga on a large scale2O3A film.

Description

Preparation method of high-quality kappa-phase gallium oxide epitaxial film
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to high-quality kappa-Ga2O3A method for preparing a film.
Background
Gallium oxide (Ga)2O3) The semiconductor material is a super-wide bandgap semiconductor material, has the characteristics of large bandgap width, high breakdown field strength, good photoelectric performance and the like, and has wide application prospect in the fields of optoelectronic devices and power semiconductor devices. Research reports that Ga2O3There are at least 5 phases of the material,are α, β, γ, κ, δ, respectively. At present, against Ga2O3Mainly focusing on the thermally stable phase beta-Ga2O3And for metastable phase kappa-Ga2O3Also less studied, the first by heating delta-Ga at 500 deg.C2O3It was found that kappa-Ga2O3。κ-Ga2O3The free energy of formation is only higher than that of beta-Ga2O3Reflecting its metastable phase behavior over a range of temperatures.
With beta-Ga2O3Same, kappa-Ga2O3The material also has the characteristics of large forbidden band width and high breakdown field strength, and the characteristics enable the material to have strong potential application value in the aspect of high-power electronic devices. Recent reports have shown that kappa-Ga is due to2O3The spontaneous polarization exists, and the theory predicts that the two-dimensional electron gas with high mobility can be formed and can be used for preparing the high electron mobility transistor. Studies have shown that kappa-Ga2O3And the ferroelectric memory has stronger ferroelectric property and has good application prospect in the aspects of ferroelectric memory devices, metal ferroelectric semiconductor transistors and the like.
At present, Ga2O3The preparation methods of (1) include metal organic chemical vapor phase epitaxy (MOCVD), Molecular Beam Epitaxy (MBE) and the like, and the methods have been proved to be capable of preparing beta-Ga with better quality2O3Thin films, however, these methods still have many problems such as slow growth rate, difficult phase control, etc. Limited by these disadvantages, in the metastable phase Ga2O3Especially in kappa-Ga2O3The research on the aspects is very little, so that the research and the application of the material properties have obvious defects.
Because of using MOCVD and MBE growth method to prepare kappa-Ga2O3Slower rate of film, kappa-Ga2O3Thick film epitaxy is difficult, and heteroepitaxy generally has poor crystal quality due to lattice mismatch, is usually accompanied by phase mixing, and is difficult to be used as a high-quality semiconductor material for preparing high-power devices, so that a fast growth method is requiredFast growth of high quality kappa-Ga2O3A method of making a thin film.
Disclosure of Invention
In order to solve the above-mentioned technical problems, it is an object of the present invention to provide a method for growing high quality κ -Ga using Halide Vapor Phase Epitaxy (HVPE)2O3The method has the advantages of high growth speed, simple device, low cost and the like, and the grown kappa-Ga2O3The crystal quality is better, and the surface roughness is low. The grown film material can be used for solar blind ultraviolet detectors and power electronic devices. Meanwhile, the material grown by the method has better uniformity, and large-area heteroepitaxy can be realized.
In order to achieve the aim, the invention provides the technical scheme that the kappa-Ga is grown by Halide Vapor Phase Epitaxy (HVPE)2O3The film forming method uses a two-temperature-zone tube furnace as reaction equipment, and high-purity metal Ga and HCl of mixed carrier gas react under the heating of a first temperature zone (reaction zone) to generate gaseous GaCl and GaCl3Then under the drive of carrier gas, the reaction product in the first temperature zone (reaction zone) enters the second temperature zone (growth zone) and mixes with O of carrier gas2Reaction, growth of kappa-Ga on substrate2O3A film. The first temperature zone (reaction zone) adopts higher temperature to react the metal Ga source and gaseous HCl, the temperature used in the first temperature zone is 800-1050 ℃, and the second temperature zone (growth zone) adopts lower temperature to ensure that the product conveyed from the first temperature zone is reacted with O2And reacting, wherein the temperature of the second temperature zone is 500-650 ℃.
The invention can be based on a halide vapor phase epitaxial growth method of a modified tubular annealing furnace. The device used in the scheme is a common tube annealing furnace structure, and an internal gas circuit is added on the basis, so that two paths of gas can be introduced into the tube annealing furnace in an internally-externally nested manner. The growth equipment is a two-temperature-zone annealing furnace through a modified gas circuit, two gas circuits are arranged inside and outside the tubular annealing furnace in an embedded mode, namely, an inner quartz tube and an outer quartz tube are adopted in the tubular annealing furnace: the inner tube can pass through the first temperature zone in length, the metal Ga source is arranged in the inner tube, and HCl gas of mixed carrier gas is introducedPut into an inner tube and react under high-temperature heating to generate GaCl and GaCl3Enters a second temperature zone under the driving of the carrier gas, a GaN or sapphire substrate is placed in the second temperature zone, oxygen of the mixed carrier gas is introduced into the second temperature zone from the outer quartz tube to react with the product of the first temperature zone, and is deposited on the substrate with low cost to form kappa-Ga2O3A film.
The gas introduced into the inner quartz tube is HCl gas as reactant and Ar or N as carrier gas2Gas, HCl to carrier gas ratio 1:10 to 1: 20, the gas introduced into the outer quartz tube is O as a reactant2Gas and Ar or N as carrier gas2Gas, O2The ratio to carrier gas is 1: 15 to 1: and 30, the ratio of the total flow of the gas introduced into the inner quartz tube to the total flow of the gas introduced into the outer quartz tube is 1:5 to 1: 10.
The substrate used in the growth is a lead-zinc-ore substrate such as sapphire or GaN.
The additionally added gas path is introduced into the annealing furnace by adopting a quartz tube, and the position of the quartz tube is used as a reaction area of the first step reaction, and the quartz tube is communicated with a growth area of the second step reaction.
Compared with the prior art, the invention has the beneficial effects that: kappa-Ga provided in the examples of the present invention2O3The film preparation facilities are modified by adopting a simple tubular annealing furnace, so that the growth process is simple and easy to control, the raw materials with low cost are adopted, the cost is low, and the reaction raw materials and the products are harmless to the environment.
kappa-Ga grown in examples of the invention2O3Is a pure phase crystal, is a high-quality finished product, and has no other phase under an X-ray diffraction pattern. kappa-Ga grown in examples of the invention2O3The growth rate was about 3 microns/hour.
kappa-Ga grown in examples of the invention2O3The full width at half maximum of the rocking curve is narrow, the density of lattice defects is low, and the lattice quality is good.
Drawings
Fig. 1 is a schematic view of a tube annealing furnace-based growth gas circuit provided in example 1.
FIG. 2 is a schematic view of the growth apparatus and growth process provided in example 1
Fig. 3 is an X-ray diffraction pattern of a sample obtained by growing on a sapphire substrate based on the modified device provided in example 1, which comprises an XRD-2 theta diagram (left figure) and a rocking graph (right figure).
Detailed description of the preferred embodiments
The invention is described below with reference to the accompanying drawings:
the invention provides a method for growing kappa-Ga2O3The method of (3), comprising retrofitting a growth apparatus and a specific growth method. According to the specific embodiment of the invention, the growth equipment is a two-temperature-zone tube annealing furnace with a modified gas circuit, an inner quartz tube and an outer quartz tube are nested in the furnace, and the gas circuit is separated by a flange of the quartz tube (figure 1), so that one path of gas can be respectively introduced into the inner quartz tube and the outer quartz tube of the growth equipment. The length of the inner tube of the growth equipment can penetrate through the first temperature zone, the metal Ga source is arranged in the inner tube, the Ga position is in the middle of the first temperature zone (reaction zone), HCl gas mixed with carrier gas is introduced into the inner tube and reacts under high-temperature heating, and generated GaCl and GaCl are generated3Driven by carrier gas, enters a second temperature zone (growth zone), a GaN or sapphire substrate is placed in the second temperature zone (growth zone), and O of the carrier gas is mixed2Reacting with the product of the first temperature zone in the second temperature zone (growth zone) and depositing on the substrate to form kappa-Ga2O3A film.
The inner layer quartz tube of the device is used as a position for placing a reactant Ga source, and reacts with HCl introduced into the inner layer quartz tube to generate GaCl and GaCl3Carried to the growth region by the introduced gas, and O2Reaction to produce kappa-Ga2O3Growing on the surface of the lead-zinc ore substrate of sapphire or GaN and the like placed in the growth region.
The invention provides a method for growing kappa-Ga by halide vapor phase epitaxy2O3The method comprises the following steps:
metal Ga is arranged in the middle of the inner-layer quartz tube, and a lead-zinc ore substrate such as sapphire or GaN is arranged in a growth region of the outer-layer quartz tube, wherein the distance from the end of the inner-layer quartz tube is 0-30 cm.
The substrate is vertically placed on the support, so that the growth on the substrate is more uniform.
And opening a tubular furnace heating system, heating the reaction zone where the metal Ga is positioned to 800-1050 ℃, and heating the growth zone where the substrate is positioned to 500-600 ℃.
And stopping introducing the gas after the growth process is carried out for a specified time, and closing the heating system to naturally cool the tubular annealing furnace. After the growth process is carried out for a specified time, the heating system is closed, and only HCl and O are stopped from being introduced2While continuing to introduce carrier gas N2Or Ar, and the quality of the product is prevented from being uncontrollable due to the fact that residual gas in the tube continues to react and grow.
And taking out the grown sample, and cleaning and airing the sample.
According to the specific embodiment of the invention, the reaction growth is carried out by simultaneously introducing the reaction gas into the inner quartz tube and the outer quartz tube, wherein the gas introduced into the inner quartz tube is HCl gas as a reactant and Ar or N as a carrier gas2Gas, HCl to carrier gas ratio 1:10 to 1: 20, the reaction temperature of HCl and Ga is 800-1050 ℃. Ar gas is used as a carrier gas for the reaction, instead of N2Prevent N2In which other possible reactions take place.
The gas introduced into the outer quartz tube is O as a reactant2Gas and Ar or N as carrier gas2Gas, O2The ratio to carrier gas is 1: 15 to 1: 30, O2The reaction temperature of the product in the first temperature zone in the second temperature zone is 500-650 ℃, and the ratio of the total flow of the gas introduced into the inner tube to the total flow of the gas introduced into the outer tube is 1:5 to 1: 10; HCl and O are introduced2The ratio of (A) to (B) is not more than 1:4, and the total time of introducing the reaction gas during growth is not less than 5 minutes.
According to the embodiment of the present invention, the substrate used in the growth is a sapphire or GaN or other lead-zincite substrate, and preferably, β -Ga may be used2O3The substrate is homoepitaxial.
According to a particular embodiment of the invention, the kappa-Ga is grown2O3The thickness of the film is 0.1-5 um.
Example 1: this example provides a hetero-epitaxial growth of kappa-Ga on the surface of a sapphire substrate2O3The method comprises the step of modifying the growth equipment and a specific growth method, wherein the modification of the growth equipment is shown in figure 1, and the overall growth principle schematic diagram is shown in figure 2.
In the gas circuit structure of embodiment 1 shown in fig. 1, the flange 11 is used for sealing the outer quartz tube 15 and simultaneously has a supporting function, the flange 11 is provided with a second gas circuit tube 13, and O is introduced from the gas circuit tube 132With carrier gas into the outer quartz tube 15. The edge of the tube 12 is provided with a flange for sealing the inner side quartz tube and simultaneously playing a supporting role, the tube 12 is communicated with the first gas path tube 14, and HCl and carrier gas are introduced into the inner side quartz tube from the first gas path tube 14. The inner quartz tube and the outer quartz tube do not communicate at this side. The tube 12 leads to the right inner tube 16, which is provided with a growth substrate 17 on the outside. The outer quartz tube 15 is sleeved outside the right inner tube 16. The heating may be carried out by wrapping the heating element 18 around a tube in which the temperature sensing device is located.
FIG. 2 is a schematic view of the whole apparatus and reaction of example 1, in which the first temperature zone of the reaction, i.e., the reaction zone, is provided on the left side, the Ga source is disposed in the region of the inner quartz tube, in which the temperature is set to 850 ℃, and the second temperature zone of the reaction, i.e., the growth zone, is provided on the right side, in which the substrate 17 (which may be provided with the substrate holder 20) is disposed in the region of the outer quartz tube, in which the temperature is set to 550 ℃.
Taking the above device as the growth equipment of the present example, the specific operation steps are as follows:
and placing metal Ga as a reaction source material in the middle of the first temperature zone of the inner quartz tube, and placing a substrate at the position 5cm away from the inner quartz tube in the second temperature zone of the outer quartz tube. Preferably, the sapphire substrate may be placed vertically, and then the growth apparatus is brought to the temperature as described above to start heating. After the heating is completed, the temperature is stabilized for a period of time, and reaction gas is introduced, and the reaction equation of the above method is as follows:
2Ga+6HCl＝2GaCl3+3H2
2Ga+2HCl＝2GaCl+H2
4GaCl3+3O2＝2Ga2O3+6Cl2
4GaCl+3O2＝2Ga2O3+2Cl2
and (3) performing X-ray diffraction pattern characterization on the generated material, including an XRD-2 theta diagram (left diagram) and a rocking curve diagram (right diagram), and proving that the material has better single crystal purity and fewer lattice defects.
The X-ray diffraction pattern of this example is shown in figure 3.

Claims (5)

1. Method for growing kappa-Ga by adopting halide vapor phase epitaxy2O3The method is characterized in that a two-temperature-zone tube furnace is used as reaction equipment, and high-purity metal Ga and HCl mixed with carrier gas react under the heating of a first-temperature-zone reaction zone to generate gaseous GaCl and GaCl3Then under the push of carrier gas, the reaction product in the first temperature area reaction area enters the second temperature area growth area and mixes with the O of carrier gas2Reaction, growth of kappa-Ga on substrate2O3A film; the first temperature zone adopts higher temperature to make metal Ga source and gaseous HCl react, the temperature used in the first temperature zone is 800-1050 ℃, and the second temperature zone adopts lower temperature to make the product and O transported from the first temperature zone2Reacting, wherein the temperature used in the second temperature zone is 500-650 ℃; the tube furnace adopts an inner quartz tube and an outer quartz tube which are nested, the length of the inner tube can pass through the first temperature zone, the metal Ga source is arranged in the inner tube, HCl gas mixed with carrier gas is introduced into the inner tube and reacts under high-temperature heating, and generated GaCl and GaCl are generated3Enters a second temperature zone under the driving of the carrier gas, a GaN or sapphire substrate is placed in the second temperature zone, the oxygen of the mixed carrier gas reacts with the product of the first temperature zone in the second temperature zone and is deposited on the substrate to form kappa-Ga2O3A film.
2. Growing kappa-Ga according to claim 12O3Method for making thin filmAnd the substrate in the second temperature zone is a GaN or sapphire substrate.
3. Growing kappa-Ga according to claim 12O3The method for preparing the thin film is characterized in that the gas introduced into the inner quartz tube is HCl gas serving as a reactant and Ar or N2 gas serving as a carrier gas, and the ratio of HCl to the carrier gas is 1:10 to 1: 20, the gas introduced into the outer quartz tube is O as a reactant2Gas and Ar or N2 gas, O, as carrier gas2The ratio to carrier gas is 1: 15 to 1: and 30, the ratio of the total flow of the gas introduced into the inner quartz tube to the total flow of the gas introduced into the outer quartz tube is 1:5 to 1: 10.
4. Growing kappa-Ga according to one of claims 1 to 32O3The method of the film is characterized in that the gas introduced into the outer quartz tube is O as a reactant2Gas and Ar or N as carrier gas2Gas, O2The ratio to carrier gas is 1: 15 to 1: 30, O2The reaction temperature of the product in the first temperature zone in the second temperature zone is 500-650 ℃; the ratio of the total flow of the gas introduced into the inner pipe to the total flow of the gas introduced into the outer pipe is 1:5 to 1: 10; HCl and O are introduced2The ratio of (A) to (B) is not more than 1:4, and the total time of introducing the reaction gas during growth is not less than 5 minutes.
5. Growing kappa-Ga according to claim 42O3Method for thin film, characterized in that the substrate is placed vertically on a support.
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