CN116053120B - Nitride epitaxial structure and preparation method and application thereof - Google Patents

Nitride epitaxial structure and preparation method and application thereof Download PDF

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CN116053120B
CN116053120B CN202310327920.3A CN202310327920A CN116053120B CN 116053120 B CN116053120 B CN 116053120B CN 202310327920 A CN202310327920 A CN 202310327920A CN 116053120 B CN116053120 B CN 116053120B
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nitride
graphene layer
silicon carbide
graphene
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王钰宁
徐俞
徐建喜
王建峰
徐科
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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Abstract

The invention discloses a nitride epitaxial structure and a preparation method and application thereof. The preparation method comprises the following steps: firstly, forming a silicon carbide film on the surface of a substrate; converting at least a surface layer region of the silicon carbide film to form a graphene layer; and growing a nitride monocrystal on the surface of the graphene layer to form a nitride epitaxial structure. The preparation method of the nitride epitaxial structure provided by the invention can be used for epitaxial high-quality monocrystal gallium nitride on a monocrystal or polycrystal substrate, and the heat radiation performance of a gallium nitride-based HEMT device is improved.

Description

Nitride epitaxial structure and preparation method and application thereof
Technical Field
The invention particularly relates to a nitride epitaxial structure, a preparation method and application thereof, and belongs to the technical field of semiconductors.
Background
Gallium nitride (GaN), aluminum nitride (AlN) and other wide bandgap semiconductor materials are used as representatives of third-generation semiconductor materials, have the advantages of high breakdown field strength, heat conductivity, electron mobility and the like, are core bases of new-generation photoelectrons, power electrons and high-frequency microelectronics in the future, and are ideal materials for preparing photoelectric devices and high-power electronic devices. Gallium nitride (GaN) is used as a third-generation semiconductor material, has the advantages of high breakdown field strength, high thermal conductivity, high electron mobility and the like, and is widely applied to the aspects of microwave radio frequency, semiconductor illumination, power electronic devices and the like. Gallium nitride-based High Electron Mobility Transistors (HEMTs) are considered to be ideal devices for high frequency, high power amplifiers required for next generation communication technologies based on the inherent characteristics of gallium nitride materials and the formation of two-dimensional electron gases at the AlGaN/GaN heterojunction interface. AlGaN/GaN HEMTs have been demonstrated to be capable of 20W mm in the X band -1 Is operated at a speed of (3).
Typically, gallium nitride is a material selected from the group consisting of silicon (Si), sapphire (Al 2 O 3 ) Heteroepitaxially grown on these substrates, but with low thermal conductivity (Si-130W m) -1 ·K -1 ，Al 2 O 3 ~ 40 W·m -1 ·K -1 ) Resulting in nitride-based semiconductor devicesThe heat dissipation performance is poor, and due to larger lattice mismatch and thermal mismatch in heterogeneous epitaxy, larger stress, defects and even cracks are usually generated in the epitaxial growth of nitride, so that the performance of subsequent devices is seriously affected. When the device is in a high bias voltage working state, excessive power dissipation leads to device temperature rise, and the traditional low-heat conductivity substrate and a heat dissipation path have limited heat dissipation capability, so that heat is prevented from diffusing to the surrounding environment, further phonon scattering is enhanced, carrier mobility in a potential well is reduced, static I-V characteristics of the device are attenuated, the phenomenon is called self-heating effect, and the application of the nitride semiconductor device under a high power condition is severely limited.
Diamond has the highest thermal conductivity in nature (more than 2000W m at room temperature) -1 ·K -1 ) The self-heating effect of the device can be effectively improved, and the reliability and performance of the device can be improved. However, single crystal diamond is a cubic crystal, gallium nitride used for power device fabrication is a hexagonal crystal, and (0001) gallium nitride is intended to be directly epitaxially grown on diamond, and (111) plane diamond is selected as a substrate. There are also difficulties in epitaxially growing gallium nitride material on (111) plane diamond substrates. On one hand, the (111) plane diamond substrate is difficult to grow and expensive, so that the whole manufacturing cost of the device is high; on the other hand, gallium nitride has large lattice mismatch and thermal mismatch with diamond, and it is difficult to obtain high quality gallium nitride material.
In recent years, more and more attention has been focused on two-dimensional materials such as graphene, hexagonal boron nitride (h-BN), transition Metal Dihalide Carbon (TMDC), and the like. Among the various two-dimensional materials, graphene offers promising properties for use as a substrate, such as high conductivity, excellent mechanical strength, optical transparency, amphoteric doping, and large-area production, and has been found to receive a great deal of attention since 2004. Nitride is grown on graphene, so-called quasi-van der Waals epitaxy (QvdwE), which is a non-corresponding epitaxial mode, i.e., the epitaxial layer and the substrate are not strictly lattice-matched, so that the strain caused by interface lattice mismatch can be relieved by using weak van der Waals force of an interface, and the defect density is reduced to obtain a nitride material with low stress and low defect density. In addition, nitride materials grown on graphene can be obtained only through simple mechanical stripping, a power device with high heat dissipation performance can be prepared by transferring the nitride materials onto a metal substrate, and foldable display can be realized by transferring the nitride materials onto a flexible substrate.
Currently, most of the graphene used in QvdwE technology is transferred to an epitaxial substrate after a metal substrate (such as copper, nickel, platinum, etc.) is grown by Chemical Vapor Deposition (CVD). For graphene with the thickness of only atoms or a few nanometers, the graphene is extremely easy to damage and form wrinkles in the transfer process due to low overall strength, and the PMMA transfer glue residues exist, so that the crystal quality of the subsequent epitaxial nitride is seriously affected. In addition, graphene can be directly formed on the surface through high-temperature sublimation of the SiC substrate, so that QvdwE of subsequent nitrides can be performed. The graphene prepared by the method does not need to be transferred, but the self-supporting SiC substrate is high in price, and is unfavorable for the wide application of QvdwE technology.
Disclosure of Invention
The invention mainly aims to provide a nitride epitaxial structure, and a preparation method and application thereof, thereby overcoming the defects in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
in one aspect, the present invention provides a method for preparing a nitride epitaxial structure, including:
firstly, forming a silicon carbide film on the surface of a substrate;
converting at least a surface layer region of the silicon carbide film to form a graphene layer;
and growing a nitride monocrystal on the surface of the graphene layer to form a nitride epitaxial structure.
Further, the preparation method specifically comprises the following steps: and (3) annealing the silicon carbide film at the temperature of 1200-1650 ℃ for 5-300min so as to convert at least the surface layer region of the silicon carbide film into a graphene layer, wherein after the annealing is finished, the region from the surface to the set depth of the silicon carbide film is converted into the graphene layer, and the rest part is reserved and the silicon carbide layer is formed.
Specifically, the number of layers of the formed graphene layer can be controlled by controlling the temperature and time of the annealing treatment, for example, when the temperature of the annealing treatment is 1200-1650 ℃ and the time is 5-60min, the formed graphene layer is single-layer graphene, when the temperature of the annealing treatment is 1200-1650 ℃ and the time is 60-150min, the formed graphene layer is 2-layer graphene, and when the temperature of the annealing treatment is 1200-1650 ℃ and the time is 150-300min, the formed graphene layer is more than 3 layers of graphene.
Further, the preparation method specifically comprises the following steps: at least the surface layer region of the silicon carbide film is converted into single-layer graphene, when the graphene layer is single-layer graphene, the electrostatic potential of the silicon carbide layer can penetrate through the graphene layer, and the electrostatic potential can penetrate through the graphene to generate orientation guidance on the nitride single crystal, so that the orientation and the polarity of the nitride single crystal are matched with the lattice information of the composite substrate comprising the silicon carbide layer and the substrate, and the quality of the nitride single crystal is better.
Specifically, direct epitaxy of a nitride single crystal on a hetero-substrate such as diamond is heteroepitaxy, and there are problems of large lattice mismatch and thermal mismatch due to the difference in lattice constant and thermal expansion coefficient between the hetero-substrate such as diamond and nitride such as gallium nitride, whereas when nitride is epitaxially grown on graphene, nitride and graphene are not connected by covalent bonds but are not connected by van der Waals force, which is a weak interaction force, so that misfit dislocation caused by lattice mismatch and thermal mismatch can be alleviated, and stress can be reduced, and specifically, the dislocation density of GaN is lowered as the dislocation density of an aluminum nitride buffer layer is lowered, because dislocation of AlN is extended upward into GaN during epitaxy.
More specifically, the orientation and polarity of the nitride single crystal are identical to those of the silicon carbide layer. For example, when single-layer graphene is formed on the surface layer of the SiC layer with the orientation of (0001) and the Si polarity, the out-of-plane orientation and the polarity of AlN formed by growth on the single-layer graphene will be (0001) and the AlN polarity, and the in-plane orientation will be identical to that of the SiC layer, that is, as the result of directly heteroepitaxial AlN on the SiC substrate, the electrostatic potential penetration effect of the SiC layer on the single-layer graphene can enhance the van der waals force of the interface, realize the epitaxy with strong interface interaction, and will not generate misfit dislocation, thereby realizing the "remote epitaxy" of the nitride single crystal.
Further, the thickness of the graphene layer is 0.34-34nm, preferably 1-27 nm, and the thickness of the silicon carbide layer is 2-2000 nm.
Further, the preparation method specifically comprises the following steps: and growing a monocrystalline aluminum nitride buffer layer and a monocrystalline gallium nitride layer on the surface of the graphene layer in sequence so as to form the nitride epitaxial structure, or growing a monocrystalline aluminum nitride layer or a monocrystalline gallium nitride layer on the surface of the graphene layer so as to form the nitride epitaxial structure.
Further, the preparation method specifically comprises the following steps: placing a substrate with a graphene layer formed on the surface in a reaction chamber, introducing a nitrogen source and an aluminum source into the reaction chamber at the temperature of 1000-1200 ℃, controlling the introduction rate of the aluminum source to be 50-100 sccm and the introduction rate of the nitrogen source to be 0.5-2 slm, so as to grow on the surface of the graphene layer to form a monocrystal aluminum nitride buffer layer; introducing a nitrogen source and a gallium source into the reaction chamber at the temperature of 1000-1100 ℃, controlling the introducing speed of the gallium source to be 0-100 sccm and the introducing speed of the nitrogen source to be 8-15 slm, so as to grow and form a monocrystalline gallium nitride layer on the surface of the monocrystalline aluminum nitride buffer layer;
or placing the substrate with the graphene layer formed on the surface in a reaction chamber, introducing a nitrogen source and an aluminum source into the reaction chamber at 900-1700 ℃, controlling the introducing rate of the aluminum source to be 50-100 sccm and the introducing rate of the nitrogen source to be 0.5-2 slm, so as to grow and form a monocrystal aluminum nitride layer on the surface of the graphene layer;
or placing the substrate with the graphene layer formed on the surface in a reaction chamber, introducing a nitrogen source and a gallium source into the reaction chamber at 600-1200 ℃, controlling the introducing speed of the gallium source to be 0-100 sccm and the introducing speed of the nitrogen source to be 8-15 slm, and thus growing a monocrystalline gallium nitride layer on the surface of the graphene layer.
Further, the preparation method further comprises the following steps: and carrying out surface treatment on the graphene layer by at least adopting oxygen-containing plasma, nitrogen-containing plasma or ammonia gas, and then growing a nitride monocrystal on the graphene layer.
Specifically, when the number of layers of the graphene layer is more than two, van der waals with weak interfaces can cause grain boundary defects in the nitride single crystal to generate dislocation, and the graphene layer is subjected to surface treatment by oxygen-containing plasma, nitrogen-containing plasma or ammonia gas, so that C-O dangling bonds can be formed in the graphene layer, and the nitride single crystal and the graphene layer are combined through the dangling bonds, thereby relieving mismatching dislocation caused by lattice mismatch and thermal mismatch, reducing the grain boundary defects, reducing dislocation density and the like.
Specifically, the growth rate of the nitride single crystal on the single-layer graphene is about 0.9 times that of the two or more layers of graphene without plasma treatment, and the growth rate of the nitride single crystal on the two or more layers of graphene after plasma treatment is improved by 1.5 times compared with that of the single crystal without plasma treatment.
Specifically, an oxygen-containing plasma is adopted to perform surface treatment on the graphene layer, a C-O suspension bond is formed in the graphene layer, then a monocrystalline aluminum nitride buffer layer is grown on the surface of the graphene layer, and Al in the monocrystalline aluminum nitride buffer layer is combined with the C-O suspension bond to form a C-O-Al bond; or, firstly adopting nitrogen-containing plasma or ammonia gas to carry out surface treatment on the graphene layer, forming a C-N suspension bond in the graphene layer, then growing a monocrystalline aluminum nitride buffer layer on the surface of the graphene layer, wherein Al in the monocrystalline aluminum nitride buffer layer is combined with the C-N suspension bond to form a C-N-Al bond, and correspondingly, when a monocrystalline gallium nitride layer grows on the surface of the graphene layer, ga in the monocrystalline gallium nitride layer can be combined with the C-O suspension bond to form a C-O-Ga bond and combined with the C-N suspension bond to form a C-N-Ga bond.
Further, the surface treatment of the graphene layer by oxygen-containing plasma is carried out with the radio frequency power of 50-150mW and the treatment time of 20-60s; the surface treatment of the graphene layer by using the nitrogen-containing plasma is carried out by adopting radio frequency power of 50-150W and the treatment time of 10-60s.
Further, the substrate includes a diamond substrate or a sapphire substrate, which may be a patterned sapphire substrate, for example, a nano-patterned sapphire substrate, or the like.
In another aspect, the present invention also provides a nitride epitaxial structure, which is obtained by the preparation method.
The invention further provides a gallium nitride-based HEMT device, which comprises the nitride epitaxial structure.
Compared with the prior art, the invention has the advantages that: the preparation method of the nitride epitaxial structure provided by the invention can be used for epitaxial high-quality nitride single crystals on a single crystal or polycrystalline substrate, and improves the heat dissipation performance of a gallium nitride-based HEMT device.
Drawings
FIG. 1 is a flow chart of a process for fabricating a nitride epitaxial structure according to an exemplary embodiment of the present invention;
FIG. 2 is a schematic illustration of a process flow for fabricating a nitride epitaxial structure according to an exemplary embodiment of the present invention;
fig. 3 is a schematic cross-sectional view of a nitride epitaxial structure a according to embodiment 1 of the present invention;
fig. 4 is a schematic structural diagram of a gallium nitride-based HEMT device according to embodiment 1 of the present invention;
fig. 5 is a schematic cross-sectional view of a nitride epitaxial structure B according to embodiment 2 of the present invention;
fig. 6 is a schematic cross-sectional view of a nitride epitaxial structure C according to embodiment 3 of the present invention;
fig. 7 is a schematic cross-sectional view of a nitride epitaxial structure D according to embodiment 4 of the present invention;
fig. 8 is a schematic cross-sectional view of a nitride epitaxial structure E according to comparative example 1 of the present invention;
fig. 9 is a schematic cross-sectional structure of a nitride epitaxial structure F according to comparative example 2 of the present invention.
Detailed Description
In view of the shortcomings in the prior art, the inventor of the present invention has long studied and practiced in a large number of ways to propose the technical scheme of the present invention. The technical scheme, the implementation process, the principle and the like are further explained as follows.
The invention provides a preparation method of a nitride epitaxial structure, which comprises the steps of sputtering a silicon carbide film on the surface of a substrate in advance, adopting high-temperature annealing to improve the crystal quality of the sputtered silicon carbide layer, forming a graphene layer on the surface layer area of the silicon carbide layer, taking the silicon carbide layer and the graphene layer as an epitaxial intermediate layer, and finally obtaining a high-quality monocrystalline gallium nitride film through epitaxy.
The technical scheme, implementation process and principle thereof, etc. will be further explained with reference to the drawings and specific embodiments, and unless otherwise indicated, sputtering processes and apparatuses, semiconductor epitaxial apparatuses, annealing apparatuses, etc. used in the embodiments of the present invention are known to those skilled in the art.
Example 1
Referring to fig. 1, a method for preparing a nitride epitaxial structure based on a diamond substrate may include the following steps:
s1: a diamond substrate is prepared. Specifically, the diamond substrate may be a polycrystalline diamond substrate and a (100) -sided, (110) -sided single crystal diamond substrate.
S2: and growing a silicon carbide layer. The method specifically comprises the following steps: a silicon carbide layer with the thickness of 60 nm is manufactured and formed on the surface of a diamond substrate by adopting a magnetron sputtering mode, wherein the sputtering temperature is 20-700 ℃, the radio frequency power is 50-200W, the target material for growing the silicon carbide layer is a Si target, and the working gases are Ar and CH 4 Alternatively, the target material for growing the silicon carbide layer can also be a SiC target, and the working gas is Ar.
S3: and growing a graphene layer. The method specifically comprises the following steps: and carrying out high-temperature annealing treatment on the silicon carbide layer at 1500 ℃ for 70min so as to completely decompose the silicon carbide and convert the silicon carbide in the surface layer region of the silicon carbide layer into two layers of graphene, thereby forming a graphene layer with the thickness of 0.7 nm.
S4: and growing an aluminum nitride buffer layer. The method specifically comprises the following steps: the epitaxial material obtained in the step S3 can be placed in a reaction chamber of an epitaxial growth device such as chemical vapor deposition and the like, the growth temperature in the reaction chamber is controlled to be 1000-1200 ℃, an aluminum source and a nitrogen source are introduced into the reaction chamber, the introduction rate of the aluminum source is controlled to be 50-100 sccm, the introduction rate of the nitrogen source is controlled to be 0.5-2 slm, and the introduction rate of the nitrogen source is kept to be 0.5-2 h, so that an aluminum nitride buffer layer with the thickness of 100-200nm is formed on the surface of the graphene layer in a growing mode.
S5: and growing a monocrystalline gallium nitride film. The method specifically comprises the following steps: and regulating the growth temperature in the reaction chamber to 1000-1100 ℃, introducing a gallium source and a nitrogen source into the reaction chamber, controlling the introducing speed of the gallium source to be 0-100 sccm, controlling the introducing speed of the nitrogen source to be 8-15 slm, and keeping the introducing speed of the nitrogen source to be 1-3 h, so that a gallium nitride layer with the thickness of 500-2000nm is grown on the surface of the aluminum nitride buffer layer, and finally obtaining a nitride epitaxial structure based on the diamond substrate, wherein the structure A is shown in fig. 3, the nitride epitaxial structure based on the diamond substrate is processed into a gallium nitride HEMT device by adopting a semiconductor processing technology, and the structure of the device A is shown in fig. 4.
Example 2
Referring to fig. 1, a method for preparing a nitride epitaxial structure based on a diamond substrate may include the following steps:
s1: a diamond substrate is prepared. Specifically, the diamond substrate may be a polycrystalline diamond substrate and a (100) -sided, (110) -sided single crystal diamond substrate.
S2: and growing a silicon carbide layer. The method specifically comprises the following steps: a silicon carbide layer with the thickness of 50nm is manufactured and formed on the surface of a diamond substrate by adopting a magnetron sputtering mode, wherein the sputtering temperature is 20-700 ℃, the radio frequency power is 50-200W, the target material for growing the silicon carbide layer is a Si target, and the working gases are Ar and CH 4 Alternatively, the target material for growing the silicon carbide layer can also be a SiC target, and the working gasThe body is Ar.
S3: and growing a graphene layer. The method specifically comprises the following steps: carrying out high-temperature annealing treatment on the silicon carbide layer at 1300 ℃ for 5min so as to completely decompose the silicon carbide and convert the silicon carbide in the surface layer area of the silicon carbide layer into single-layer graphene, thereby forming a graphene layer with the thickness of 0.34 nm; when the formed graphene has only one layer, the electrostatic potential of the SiC layer after the reservation can penetrate through the graphene and guide the orientation and the polarity of the epitaxial AlN buffer layer to follow the lattice information of the substrate, so that the monocrystalline AlN film can be obtained, and the quality of the obtained nitride is better.
S4: and growing an aluminum nitride buffer layer. The method specifically comprises the following steps: the epitaxial material obtained in the step S3 can be placed in a reaction chamber of an epitaxial growth device such as chemical vapor deposition and the like, the growth temperature in the reaction chamber is controlled to be 1000-1200 ℃, an aluminum source and a nitrogen source are introduced into the reaction chamber, the introduction rate of the aluminum source is controlled to be 50-100 sccm, the introduction rate of the nitrogen source is controlled to be 0.5-2 slm, and the introduction rate of the nitrogen source is kept to be 0.5-2 h, so that an aluminum nitride buffer layer with the thickness of 90-180nm is formed on the surface of the graphene layer in a growing mode.
S5: and growing a monocrystalline gallium nitride film. The method specifically comprises the following steps: and regulating the growth temperature in the reaction chamber to 1000-1100 ℃, introducing a gallium source and a nitrogen source into the reaction chamber, controlling the introducing speed of the gallium source to be 0-100 sccm, controlling the introducing speed of the nitrogen source to be 8-15 slm, and keeping 1-3 h, so that a gallium nitride layer with the thickness of 500-2000nm is grown on the surface of the aluminum nitride buffer layer, and finally obtaining a nitride epitaxial structure based on the diamond substrate, wherein the structure B is shown as a structure B, a gallium nitride HEMT device is formed by processing the nitride epitaxial structure based on the diamond substrate by adopting a semiconductor processing technology, and the structure of the device B is shown as a device B, and the structure of the device B is shown as a structure in reference to fig. 4.
Example 3
Referring to fig. 1, a method for preparing a nitride epitaxial structure based on a diamond substrate may include the following steps:
s1: a diamond substrate is prepared. Specifically, the diamond substrate may be a polycrystalline diamond substrate and a (100) -sided, (110) -sided single crystal diamond substrate.
S2: and growing a silicon carbide layer. The method specifically comprises the following steps: a silicon carbide layer with the thickness of 40nm is manufactured and formed on the surface of a diamond substrate by adopting a magnetron sputtering mode, wherein the sputtering temperature is 20-700 ℃, the radio frequency power is 50-200W, the target material for growing the silicon carbide layer is a Si target, and the working gases are Ar and CH 4 Alternatively, the target material for growing the silicon carbide layer can also be a SiC target, and the working gas is Ar.
S3: and growing a graphene layer. The method specifically comprises the following steps:
1) Carrying out high-temperature annealing treatment on the silicon carbide layer at 1600 ℃ for 240min so as to completely decompose the silicon carbide and convert the silicon carbide in the surface layer area of the silicon carbide layer into four layers of graphene, thereby forming a graphene layer;
2) And carrying out surface treatment on the graphene layer by adopting oxygen-containing plasma for 40s, wherein the radio frequency power adopted by the oxygen-containing plasma is 100mw, and C-O dangling bonds are formed in the graphene layer.
S4: and growing an aluminum nitride buffer layer. The method specifically comprises the following steps: the epitaxial material obtained in the step S3 can be placed in a reaction chamber of an epitaxial growth device such as chemical vapor deposition and the like, the growth temperature in the reaction chamber is controlled to be 1000-1200 ℃, an aluminum source and a nitrogen source are introduced into the reaction chamber, the introduction rate of the aluminum source is controlled to be 50-100 sccm, the introduction rate of the nitrogen source is controlled to be 0.5-2 slm, and the introduction rate of the nitrogen source is kept to be 0.5-2 h, so that an aluminum nitride buffer layer with the thickness of 150-300nm is formed on the surface of the graphene layer, and in the process of forming the aluminum nitride buffer layer, al in the aluminum nitride buffer layer is combined with a C-O suspension bond to form a C-O-Al bond, so that the nucleation site for the subsequent aluminum nitride growth is increased, and the growth rate and the crystal quality of aluminum nitride are improved.
S5: and growing a monocrystalline gallium nitride film. The method specifically comprises the following steps: and regulating the growth temperature in the reaction chamber to 1000-1100 ℃, introducing a gallium source and a nitrogen source into the reaction chamber, controlling the introducing speed of the gallium source to be 0-100 sccm, controlling the introducing speed of the nitrogen source to be 8-15 slm, and keeping the introducing speed of the nitrogen source to be 1-3 h, so that a gallium nitride layer with the thickness of 500-2000nm is grown on the surface of the aluminum nitride buffer layer, finally obtaining a nitride epitaxial structure based on a diamond substrate, namely a structure C, wherein the structure C is shown in fig. 6, and a gallium nitride-based HEMT device is formed by processing the nitride epitaxial structure based on the diamond substrate by adopting a semiconductor processing technology, and is shown as a device C, and the structure of the device C is shown in fig. 4.
Example 4
Referring to fig. 1 and 2, a method for preparing a nitride epitaxial structure based on a diamond substrate may include the following steps:
s1: a diamond substrate is prepared. Specifically, the diamond substrate may be a polycrystalline diamond substrate and a (100) -sided, (110) -sided single crystal diamond substrate.
S2: and growing a silicon carbide layer. The method specifically comprises the following steps: a silicon carbide layer with the thickness of 50nm is manufactured and formed on the surface of a diamond substrate by adopting a magnetron sputtering mode, wherein the sputtering temperature is 20-700 ℃, the radio frequency power is 50-200W, the target material for growing the silicon carbide layer is a Si target, and the working gases are Ar and CH 4 Alternatively, the target material for growing the silicon carbide layer can also be a SiC target, and the working gas is Ar.
S3: and growing a graphene layer. The method specifically comprises the following steps: and carrying out high-temperature annealing treatment on the silicon carbide layer at 1500 ℃ for 300min so as to completely decompose the silicon carbide and completely convert the silicon carbide layer into multi-layer graphene, thereby forming the graphene layer.
S4: and growing an aluminum nitride buffer layer. The method specifically comprises the following steps: the epitaxial material obtained in the step S3 can be placed in a reaction chamber of an epitaxial growth device such as chemical vapor deposition and the like, the growth temperature in the reaction chamber is controlled to be 1000-1200 ℃, an aluminum source and a nitrogen source are introduced into the reaction chamber, the introduction rate of the aluminum source is controlled to be 50-100 sccm, the introduction rate of the nitrogen source is controlled to be 0.5-2 slm, and the introduction rate of the nitrogen source is kept to be 0.5-2 h, so that an aluminum nitride buffer layer with the thickness of 100-200nm is formed on the surface of the graphene layer in a growing mode.
S5: and growing a monocrystalline gallium nitride film. The method specifically comprises the following steps: and adjusting the growth temperature in the reaction chamber to 1000-1100 ℃, introducing a gallium source and a nitrogen source into the reaction chamber, controlling the introducing speed of the gallium source to be 0-100 sccm, controlling the introducing speed of the nitrogen source to be 8-15 slm, and keeping 1-3 h, so that a gallium nitride layer with the thickness of 500-2000nm is grown on the surface of the aluminum nitride buffer layer, and finally obtaining a nitride epitaxial structure based on the diamond substrate, wherein the structure D is shown as a structure D, a gallium nitride HEMT device is formed by processing the nitride epitaxial structure based on the diamond substrate by adopting a semiconductor processing technology, and the structure of the device D is shown as a device D, and the structure of the device D is shown as a structure in reference to fig. 4.
Example 5
Referring to fig. 1, a method for preparing a nitride film based on a sapphire substrate may include the following steps:
s1: a substrate is prepared. The substrate comprises sapphire (Al 2 O 3 ) Patterned sapphire (PSS) or nano-patterned sapphire (NPSS).
S2: and growing a silicon carbide layer. Specifically, a silicon carbide layer with the thickness of 200nm is directly formed on a substrate by epitaxial growth by adopting a CVD (chemical vapor deposition) or Molecular Beam Epitaxy (MBE) method or a magnetron sputtering technology or a Pulsed Laser Deposition (PLD) method, and the silicon carbide layer can also be obtained by adopting a transfer technology. The growth temperature of the silicon carbide film prepared by the CVD method is 1100-1600 ℃, and Si is C=1: 4-8, and pressure of 30-100 Torr. The growth temperature of the MBE method for preparing the silicon carbide film is 700-1000 ℃. Si targets can be selected for preparing silicon carbide films by using radio frequency magnetron sputtering method, and working gases are Ar and CH 4 Optionally, a SiC target is adopted, the working gas is Ar, the radio frequency power is 50-200W, the gas flow range is 0-100 sccm, and the temperature is 20-700 ℃.
S3: and generating a graphene layer. And carrying out high-temperature annealing treatment on the silicon carbide layer at 1300 ℃ for 5min so as to completely decompose the silicon carbide and convert the silicon carbide in the surface layer region of the silicon carbide layer into single-layer graphene with the thickness of 0.34nm, thereby forming the graphene layer.
S4: a nitride single crystal thin film is grown. The growth temperature of the gallium nitride film is 600-1200 ℃, and the growth temperature of the aluminum nitride film is 900-1700 ℃.
Comparative example 1
A method for manufacturing a nitride epitaxial structure based on a diamond substrate in comparative example 1 was substantially the same as in example 2, except that:
comparative example 1 is a GaN/AlGaN heterojunction material based on a single-crystal diamond substrate and a preparation method thereof disclosed in reference CN110828291a, an AlN nucleation layer is sputtered on the single-crystal diamond substrate covered with single-layer graphene by using a magnetron sputtering technique, then a low-temperature GaN transition layer is grown first at 450-600 ℃ by using an MOCVD technique, and then a GaN buffer layer is grown at 900-1000 ℃, so that the obtained nitride epitaxial structure based on the diamond substrate is denoted as structure E, the structure E is shown in fig. 8, the nitride epitaxial structure based on the diamond substrate is processed into a gallium nitride-based HEMT device by using a semiconductor processing technique, and the structure of the device E is denoted as device E, and the structure of the device E is denoted as fig. 4.
Comparative example 2
A method for manufacturing a nitride epitaxial structure based on a diamond substrate in comparative example 2 is substantially the same as in example 1 or example 2, except that:
the graphene layer in comparative example 2 was formed on the surface of a diamond substrate by using a transfer technique according to the method disclosed in CN108428618A, the finally obtained nitride epitaxial structure based on the diamond substrate was denoted as structure F, which is shown in fig. 9, and the nitride epitaxial structure based on the diamond substrate was processed to form a gallium nitride-based HEMT device by using a semiconductor processing technology, and was denoted as device F, and the structure of device F was referred to in fig. 4.
The epitaxial structures and devices in examples 1-4 and comparative examples 1-2 were respectively subjected to test characterization, and obtained through the test: structure a has a dislocation density of 5 x 10 8 cm -2 The dislocation density of structure B was 6X 10 7 cm -2 The dislocation density of structure C was 2X 10 8 cm -2 The dislocation density of structure D was 7X 10 8 cm -2 Structure E has a dislocation density of 9 x 10 8 cm -2 The dislocation density of structure F was 2X 10 9 cm -2 。
According to the preparation method of the nitride epitaxial structure, graphene is formed on the surface of the diamond substrate through high-temperature annealing of silicon carbide, the number of layers of the graphene is controllable, the structure is complete, the number of layers of the graphene corresponds to the thickness of a nitride film in the longitudinal direction of the device, and meanwhile, the in-situ conversion process avoids the damage, wrinkling, PMMA glue and other pollution problems caused by the introduction of the graphene in the transfer process; and the thermal conductivities of diamond and graphene (800-2000 w/m.k and 5300 w/m.k respectively) are higher than those of the conventional SiC (490 w/m.k) and sapphire (27 w/m.k) substrates, and the high-quality nitride single crystal can be epitaxially grown on the single crystal or polycrystalline substrate and the heat dissipation performance of the gallium nitride-based HEMT device is improved.
The invention provides a preparation method of a nitride epitaxial structure, which uses oxygen plasma, nitrogen plasma or NH 3 After the surface treatment is carried out on the graphene layer, C-O hanging bonds or C-N hanging bonds are formed in the graphene, when aluminum nitride is epitaxially grown on the graphene layer, C-O-Al bonds or C-N-Al bonds are formed at the interface of the aluminum nitride and the graphene, so that nucleation sites for subsequent growth of aluminum nitride are increased, the growth rate and the crystal quality of an aluminum nitride material are improved, and correspondingly, when gallium nitride is epitaxially grown on the graphene layer, C-O-Ga bonds or C-N-Ga bonds are formed at the interface of gallium nitride and the graphene, so that the nucleation sites for subsequent growth of gallium nitride are increased, and the growth rate and the crystal quality of the gallium nitride material are improved.
According to the preparation method of the nitride epitaxial structure, a layer of silicon carbide is sputtered on a substrate, and graphene is generated by high-temperature annealing, so that a high-quality nitride single crystal film is obtained; specifically, when the formed graphene is a layer, the electrostatic potential of the reserved silicon carbide layer can penetrate through the graphene layer and guide the orientation and polarity of the epitaxial aluminum nitride layer/gallium nitride layer to follow the lattice information of the silicon carbide layer, so that a single crystal aluminum nitride layer/single crystal gallium nitride layer is obtained, and further, the single crystal low defect density aluminum nitride layer/gallium nitride layer is obtained; meanwhile, the graphene has high thermal conductivity, and the heat radiation performance of the gallium nitride-based HEMT device can be improved.
It should be understood that the above embodiments are merely for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and implement the same according to the present invention without limiting the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.

Claims (19)

1. A method for fabricating a nitride epitaxial structure, comprising:
firstly, forming a silicon carbide film on the surface of a substrate, wherein the substrate is a diamond substrate or a sapphire substrate;
converting the surface layer region of the silicon carbide film into single-layer graphene, thereby forming a graphene layer, and retaining the rest of the silicon carbide film and forming a silicon carbide layer;
and growing a nitride monocrystal on the surface of the graphene layer to form a nitride epitaxial structure, wherein the graphene layer can be penetrated by electrostatic potential of the silicon carbide layer so as to enable the orientation and polarity of the nitride monocrystal to be matched with the lattice information of the composite substrate comprising the silicon carbide layer and the substrate.
2. The preparation method according to claim 1, characterized by comprising the following steps: annealing the silicon carbide film at the temperature of 1200-1650 ℃ to convert at least the surface layer region of the silicon carbide film into a graphene layer;
after the annealing treatment is completed, the region from the surface to the set depth of the silicon carbide film is converted into a graphene layer, and the rest is reserved and forms a silicon carbide layer.
3. The method according to claim 2, wherein the annealing treatment is carried out for a period of 5 to 60 minutes.
4. The method of manufacturing according to claim 1, characterized in that: the thickness of the graphene layer is 0.34-nm, and the thickness of the silicon carbide layer is 2-2000-nm.
5. The preparation method according to claim 1, characterized in that it comprises in particular: and growing a monocrystalline aluminum nitride buffer layer and a monocrystalline gallium nitride layer on the surface of the graphene layer in sequence so as to form the nitride epitaxial structure, or growing a monocrystalline aluminum nitride layer or a monocrystalline gallium nitride layer on the surface of the graphene layer so as to form the nitride epitaxial structure.
6. The preparation method according to claim 5, which comprises the following steps: placing a substrate with a graphene layer formed on the surface in a reaction chamber, introducing a nitrogen source and an aluminum source into the reaction chamber at the temperature of 1000-1200 ℃, controlling the introduction rate of the aluminum source to be 50-100 sccm and the introduction rate of the nitrogen source to be 0.5-2 slm, so as to grow on the surface of the graphene layer to form a monocrystal aluminum nitride buffer layer; introducing a nitrogen source and a gallium source into the reaction chamber at the temperature of 1000-1100 ℃, controlling the introducing speed of the gallium source to be 0-100 sccm and the introducing speed of the nitrogen source to be 8-15 slm, so as to grow and form a monocrystalline gallium nitride layer on the surface of the monocrystalline aluminum nitride buffer layer;
or placing the substrate with the graphene layer formed on the surface in a reaction chamber, introducing a nitrogen source and an aluminum source into the reaction chamber at 900-1700 ℃, controlling the introducing rate of the aluminum source to be 50-100 sccm and the introducing rate of the nitrogen source to be 0.5-2 slm, so as to grow and form a monocrystal aluminum nitride layer on the surface of the graphene layer;
or placing the substrate with the graphene layer formed on the surface in a reaction chamber, introducing a nitrogen source and a gallium source into the reaction chamber at 600-1200 ℃, controlling the introducing speed of the gallium source to be 0-100 sccm and the introducing speed of the nitrogen source to be 8-15 slm, and thus growing a monocrystalline gallium nitride layer on the surface of the graphene layer.
7. The method of manufacturing according to claim 5, further comprising: and carrying out surface treatment on the graphene layer by at least adopting oxygen-containing plasma, nitrogen-containing plasma or ammonia gas, forming C-O or C-N dangling bonds in the graphene layer, and then growing nitride single crystals on the graphene layer, wherein the nitride single crystals are combined with the graphene layer through the C-O or C-N dangling bonds.
8. The method of manufacturing according to claim 7, wherein: and carrying out surface treatment on the graphene layer by using oxygen-containing plasma with the power of 50-150mW and the treatment time of 20-60s.
9. The method of manufacturing according to claim 7, wherein: the power of the surface treatment of the graphene layer by using the nitrogen-containing plasma is 50-150W, and the treatment time is 10-60s.
10. A method for fabricating a nitride epitaxial structure, comprising:
firstly, forming a silicon carbide film on the surface of a substrate, wherein the substrate is a diamond substrate or a sapphire substrate;
converting the surface layer region of the silicon carbide film into more than two layers of graphene, thereby forming a graphene layer, and retaining the rest of the silicon carbide film and forming a silicon carbide layer;
at least adopting oxygen-containing plasma, nitrogen-containing plasma or ammonia gas to carry out surface treatment on the graphene layer, and forming C-O or C-N dangling bonds in the graphene layer;
and growing a nitride monocrystal on the surface of the graphene layer to form a nitride epitaxial structure, wherein the nitride monocrystal and the graphene layer are combined through the C-O or C-N suspension bond.
11. The method of manufacturing according to claim 10, wherein: and carrying out surface treatment on the graphene layer by using oxygen-containing plasma with the power of 50-150mW and the treatment time of 20-60s.
12. The method of manufacturing according to claim 10, wherein: the power of the surface treatment of the graphene layer by using the nitrogen-containing plasma is 50-150W, and the treatment time is 10-60s.
13. The preparation method according to claim 10, characterized by comprising the following steps: annealing the silicon carbide film at the temperature of 1200-1650 ℃ to convert at least the surface layer region of the silicon carbide film into a graphene layer;
after the annealing treatment is completed, the region from the surface to the set depth of the silicon carbide film is converted into a graphene layer, and the rest is reserved and forms a silicon carbide layer.
14. The method according to claim 13, wherein the annealing treatment is performed for 60 to 300 minutes.
15. The method of manufacturing according to claim 10, wherein: the thickness of the graphene layer is 0.7-34 and nm, and the thickness of the silicon carbide layer is 2-2000 and nm.
16. The preparation method according to claim 10, characterized by comprising the following steps: and growing a monocrystalline aluminum nitride buffer layer and a monocrystalline gallium nitride layer on the surface of the graphene layer in sequence so as to form the nitride epitaxial structure, or growing a monocrystalline aluminum nitride layer or a monocrystalline gallium nitride layer on the surface of the graphene layer so as to form the nitride epitaxial structure.
17. The preparation method according to claim 16, characterized by comprising the following steps: placing a substrate with a graphene layer formed on the surface in a reaction chamber, introducing a nitrogen source and an aluminum source into the reaction chamber at the temperature of 1000-1200 ℃, controlling the introduction rate of the aluminum source to be 50-100 sccm and the introduction rate of the nitrogen source to be 0.5-2 slm, so as to grow on the surface of the graphene layer to form a monocrystal aluminum nitride buffer layer; introducing a nitrogen source and a gallium source into the reaction chamber at the temperature of 1000-1100 ℃, controlling the introducing speed of the gallium source to be 0-100 sccm and the introducing speed of the nitrogen source to be 8-15 slm, so as to grow and form a monocrystalline gallium nitride layer on the surface of the monocrystalline aluminum nitride buffer layer;
or placing the substrate with the graphene layer formed on the surface in a reaction chamber, introducing a nitrogen source and an aluminum source into the reaction chamber at 900-1700 ℃, controlling the introducing rate of the aluminum source to be 50-100 sccm and the introducing rate of the nitrogen source to be 0.5-2 slm, so as to grow and form a monocrystal aluminum nitride layer on the surface of the graphene layer;
or placing the substrate with the graphene layer formed on the surface in a reaction chamber, introducing a nitrogen source and a gallium source into the reaction chamber at 600-1200 ℃, controlling the introducing speed of the gallium source to be 0-100 sccm and the introducing speed of the nitrogen source to be 8-15 slm, and thus growing a monocrystalline gallium nitride layer on the surface of the graphene layer.
18. A nitride epitaxial structure, characterized by: the nitride epitaxial structure is obtained by the production method according to any one of claims 1 to 17.
19. A gallium nitride-based HEMT device comprising the nitride epitaxial structure of claim 18.
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