CN114284397A - Method for growing high-quality aluminum nitride film on foreign substrate - Google Patents
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- CN114284397A CN114284397A CN202011036503.6A CN202011036503A CN114284397A CN 114284397 A CN114284397 A CN 114284397A CN 202011036503 A CN202011036503 A CN 202011036503A CN 114284397 A CN114284397 A CN 114284397A
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 62
- 239000000758 substrate Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 62
- 238000000137 annealing Methods 0.000 claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 9
- 238000000151 deposition Methods 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 60
- 239000010409 thin film Substances 0.000 claims description 27
- 238000009832 plasma treatment Methods 0.000 claims description 15
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 238000005092 sublimation method Methods 0.000 claims description 3
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 description 19
- 230000008901 benefit Effects 0.000 description 9
- 125000004429 atom Chemical group 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910052594 sapphire Inorganic materials 0.000 description 6
- 239000010980 sapphire Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000005012 migration Effects 0.000 description 5
- 238000013508 migration Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- 229910002601 GaN Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005401 electroluminescence Methods 0.000 description 2
- 238000001534 heteroepitaxy Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
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- 238000001953 recrystallisation Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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Abstract
The invention provides a method for growing a high-quality aluminum nitride film on a foreign substrate, which comprises the following steps: s1, growing a graphene film on the foreign substrate; s2, treating the graphene film by using plasma to form a large number of dangling bonds on the surface of the graphene film; s3, depositing an aluminum nitride film on the surface of the graphene film by metal organic chemical vapor deposition; and S4, annealing at high temperature to obtain the aluminum nitride film with smooth surface structure and low dislocation density. The method provided by the invention is simple in implementation process and is suitable for being applied to the fields of aluminum nitride film growth and manufacturing of photoelectric devices and electronic devices.
Description
Technical Field
The invention relates to the technical field of semiconductor material growth, in particular to a method for growing a high-quality aluminum nitride film on a foreign substrate.
Background
With the development of modern industry, a series of problems such as global energy crisis and atmospheric pollution are increasingly highlighted. Light Emitting Diodes (LEDs) are a new type of solid state lighting source and green light source, and are highly valued for their advantages of small size, high light efficiency, low power consumption, long life, and high environmental protection. The advantages of LED illumination are exerted, the quality of material growth is improved, and the high-quality epitaxy of aluminum nitride on a heterogeneous substrate is always concerned as a third-generation semiconductor material. Particularly, the high-quality epitaxial growth on the AlN thin film heterogeneous substrate can realize deep ultraviolet LED (DUV-LED), and can be applied to air and water purification, sterilization, biomedical instrument systems and the like. In recent years, heteroepitaxial growth of group III aluminum nitride films by Metal Organic Chemical Vapor Deposition (MOCVD) has become mainstream for the manufacture of optoelectronic devices such as Light Emitting Diodes (LEDs), and the heteroepitaxial growth of group III aluminum nitride films can only be grown on various foreign substrates such as silicon, silicon carbide (SiC) and sapphire due to the lack of large natural substrates that can be obtained at an economical cost. As the sapphire substrate mainly used for manufacturing the LED, the crystal quality can not meet the requirement of industrial production due to direct epitaxial growth because the lattice constants and the thermal expansion coefficients of the sapphire substrate and the III-group aluminum nitride epitaxial layer have larger difference. And the metal atoms of the aluminum nitride have a slow lateral migration rate in the growth process on the sapphire substrate, which leads to a long epitaxial growth time for growing a film, thereby affecting the production efficiency.
Disclosure of Invention
Technical problem to be solved
Aiming at the problems, the invention provides a method for growing a high-quality aluminum nitride film on a heterogeneous substrate, which at least partially solves the technical problems of long growth time, low quality and the like of the traditional preparation process.
(II) technical scheme
The invention provides a method for growing a high-quality aluminum nitride film on a foreign substrate, which comprises the following steps: s1, growing a graphene film on the foreign substrate; s2, treating the graphene film by using plasma to form a large number of dangling bonds on the surface of the graphene film; s3, depositing an aluminum nitride film on the surface of the graphene film by metal organic chemical vapor deposition; and S4, annealing at high temperature to obtain the aluminum nitride film with smooth surface structure and low dislocation density.
Further, the plasma treatment conditions in S2 include exposure to a nitrogen atmosphere for treatment at a power of 30-100 w for a treatment time of 30-50S.
Further, the plasma treatment in S2 includes performing plasma treatment using a glue applicator.
Further, the pressure of the chamber for MOCVD in S3 is 50-60 torr, and the temperature is 1100-1300 ℃.
Further, the high-temperature annealing in S4 includes performing the high-temperature annealing in a nitrogen atmosphere.
Further, the temperature of the high temperature annealing in S4 is not lower than 1600 ℃.
Furthermore, the high-temperature annealing time in S4 is 1-1.5 hours.
Further, the method for growing the graphene thin film in S1 includes a chemical vapor deposition method, a high temperature sublimation method.
Further, the conditions for growing the graphene thin film in S1 include: the reactants are methane and argon, the temperature is over 1200 ℃, and the time is 3-4 hours.
(III) advantageous effects
According to the invention, the graphene growing on the heterogeneous substrate is used as an insertion layer for growing the aluminum nitride film to extend the aluminum nitride film, so that the transverse migration rate of the substrate surface in the metal atom growing process is effectively improved, the aluminum nitride rapidly covers the substrate to form the film, and then the aluminum nitride/graphene/substrate structure is subjected to high-temperature annealing by combining with the application of a high-temperature annealing technology, so that the aluminum nitride film with a smooth and flat surface and good crystal quality is obtained.
Drawings
FIG. 1 schematically illustrates a flow chart of a method of growing a high quality aluminum nitride film on a foreign substrate according to an embodiment of the invention;
FIG. 2 schematically illustrates a method for growing a high quality AlN thin film on a foreign substrate according to an embodiment of the invention;
FIG. 3 schematically shows an atomic force microscope photomicrograph of graphene grown on a foreign substrate according to an embodiment of the invention;
fig. 4 schematically shows an atomic force microscope photograph of AlN nucleated on a plasma-treated graphene-covered foreign substrate, in accordance with an embodiment of the present invention;
FIG. 5 schematically shows an atomic force microscope photomicrograph of AlN film-formed on a plasma-treated graphene-covered foreign substrate, in accordance with an embodiment of the invention;
fig. 6 schematically shows an atomic force microscope photomicrograph of an AlN thin film, after a high temperature annealing process, epitaxial on a plasma-treated graphene-covered foreign substrate, in accordance with an embodiment of the present invention;
FIG. 7 schematically shows the X-ray rocking curves (0002) and before and after annealing of AlN thin film with and without graphene according to an embodiment of the invention
Peak comparison;
fig. 8 schematically shows a comparison of dislocation densities of AlN thin films with and without graphene before and after annealing, according to an embodiment of the present invention;
FIG. 9 schematically shows a graph of the electroluminescence peak intensity of a DUV-LED with and without graphene in accordance with an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings.
Graphene buffer layers are introduced to improve crystal quality and shorten epitaxy time, and graphene serves as a buffer layer for van der waals epitaxial growth of the gallium nitride thin film to overcome substantial thermal expansion coefficient and in-plane lattice constant mismatch between the aluminum nitride thin film and the sapphire substrate. Since graphene is a two-dimensional material, sp2The hexagonal arrangement of hybridized carbon atoms is similar to the (0001) c-plane of wurtzite, and the epitaxial process of aluminum nitride on graphene is not heteroepitaxy, but quasi van der waals epitaxy. Meanwhile, importantly, the migration barrier of metal atoms on the surface of graphene is extremely low, so that the number of metal atoms can be greatly increasedThe surface mobility in the growth process enables the film to rapidly migrate and connect into a film in the transverse direction in the growth process. In addition, graphene buffer layers also have some potential advantages over traditional buffer layers, such as potential heat dissipation and transferable layers, among others. Thus, the graphene is used as an insertion layer, so that the III-nitride-based aluminum photoelectric device has a plurality of benefits. However, the epitaxial study of aluminum nitride on graphene-based substrates is still in its initial stage, and a high quality aluminum nitride film cannot be obtained at present. The high-temperature annealing method is widely adopted in industrial production due to the remarkable effect of improving the quality of the aluminum nitride film, stable effect and simple operation.
Graphene grows directly on c-plane sapphire substrates to avoid cumbersome and cost-effective transfer processes, which always introduce ripples, damage and defects in the graphene film and limit practical applications. Furthermore, processing graphene in a nitrogen plasma to create dangling bonds allows aluminum nitride to form high density small-sized nucleation islands on graphene. And the AlN thin film formed by combining the thin crystal columns formed by expanding the small-size nuclear islands is easier to twist the crystal orientation in the high-temperature annealing process to unify the crystal orientation into the lowest energy state crystal orientation, so that the dislocation caused by the inconsistency of the crystal orientations is eliminated, and the aluminum nitride thin film with smooth surface and extremely low dislocation density is finally obtained. In summary, the present invention uses graphene as the insertion layer of heteroepitaxy of group III aluminum nitride (GaN and AlN) and combines the high temperature annealing technology to process the epitaxial aluminum nitride, so as to epitaxially grow an aluminum nitride film with a smooth surface and good crystal quality on the hetero-substrate.
Embodiments of the present invention provide a method for growing a high quality aluminum nitride thin film on a foreign substrate, comprising: s1, growing a graphene film on the foreign substrate; s2, treating the graphene film by using plasma to form a large number of dangling bonds on the surface of the graphene film; s3, depositing an aluminum nitride film on the surface of the graphene film by metal organic chemical vapor deposition; and S4, annealing at high temperature to obtain the aluminum nitride film with smooth surface structure and low dislocation density.
Referring to fig. 1, firstly, a uniform and complete graphene film is grown on a heterogeneous substrate material; carrying out plasma treatment on the formed graphene film growing on the heterogeneous substrate to enable a large number of dangling bonds to exist on the surface of the graphene film; growing an aluminum nitride film in MOCVD equipment; and transferring the obtained aluminum nitride/graphene/substrate structure to a high-temperature annealing furnace, then performing high-temperature annealing in a nitrogen atmosphere, and finally obtaining the aluminum nitride film with a smooth surface structure and extremely low dislocation density on the foreign substrate.
Before epitaxial growth, the graphene film layer is inserted and plasma treatment is carried out on the graphene to increase a large number of dangling bonds on the surface of the graphene, so that the aluminum nitride forms a high-density small-size nuclear island on the graphene. And the characteristic that metal atoms have low migration potential barrier on the surface of the graphene is utilized, so that the aluminum nitride quickly covers the substrate to form the film. And after epitaxial growth, transferring the aluminum nitride/graphene/substrate structure to a high-temperature annealing furnace for high-temperature annealing, wherein the aluminum nitride film is formed by combining thin crystal columns formed by expanding small-size nuclear islands, so that the thin crystal columns are easy to twist in the crystal orientation and are unified into the lowest energy state crystal orientation in the high-temperature annealing process, thereby eliminating dislocation caused by inconsistent crystal orientation, and finally obtaining the aluminum nitride film with smooth surface and extremely low dislocation density.
The high-quality epitaxial growth of the AlN thin film on the heterogeneous substrate can realize the deep ultraviolet LED, and the AlN thin film can be applied to air and water purification, sterilization, biomedical instrument systems and the like.
Based on the above embodiments, the plasma processing conditions in S2 include exposing to nitrogen atmosphere for processing with a power of 30-100 w and a processing time of 30-50S.
The plasma treatment aims at forming a large number of dangling bonds, has a good forming effect within the treatment power and treatment time range, and is beneficial to the nucleation growth of the aluminum nitride.
On the basis of the above embodiment, the plasma treatment in S2 includes plasma treatment using a dispenser.
The gluing machine has the advantages of low price and simple structure, so that the operation parameters are stable and controllable.
Based on the above embodiments, the pressure of the chamber for the MOCVD in S3 is 50 to 60torr, and the temperature is 1100 to 1300 ℃.
Metal organic chemical vapor deposition has the technical effect of promoting efficient lateral migration of group iii metal atoms within this pressure and temperature range, thereby enabling rapid incorporation of aluminum nitride core islands.
On the basis of the above embodiment, the high-temperature annealing in S4 includes performing the high-temperature annealing in a nitrogen atmosphere.
The purpose of carrying out high-temperature annealing in the nitrogen atmosphere is to ensure that the aluminum nitride is prevented from being decomposed in a high-temperature environment and the film property of the aluminum nitride can be effectively protected.
On the basis of the above embodiment, the temperature of the high-temperature annealing in S4 is not lower than 1600 ℃.
The purpose of the high temperature annealing is not lower than 1600 ℃ is that the recrystallization phenomenon of the aluminum nitride can be realized only when the temperature is higher than the temperature.
In addition to the above examples, the high temperature annealing time in S4 was 1 to 1.5 hours.
The annealing time within the range has the technical effects of ensuring that the quality of the aluminum nitride film can be improved through recrystallization and avoiding the generation of high-temperature decomposition phenomenon.
On the basis of the above embodiments, the method for growing the graphene thin film in S1 includes a chemical vapor deposition method and a high temperature sublimation method.
The method has the advantages of simplicity and stable parameters.
On the basis of the above embodiment, the conditions for growing the graphene thin film in S1 include growing graphene at a temperature of 1200 ℃ or higher for 3-4 hours by using methane and argon as reactants.
Under the condition, the method has the advantages that high-quality graphene can be stably grown, and pollution-free byproducts are generated.
The following describes the present invention in detail with an embodiment, please refer to fig. 2, which specifically includes:
fig. 2 is a schematic diagram illustrating a process of obtaining high-quality AlN through annealing after AlN is densely nucleated on a heterogeneous substrate covered with graphene processed by nitrogen plasma and then grown into a thin film. S31, carrying out MOCVD growth on the graphene-covered substrate subjected to the plasma treatment to obtain an aluminum nitride nuclear island; s32, continuously growing an aluminum nitride nuclear island grown by MOCVD on the substrate covered by the graphene after the plasma treatment into a film; s41, annealing the aluminum nitride film grown on the substrate covered by the graphene, wherein the thin crystal columns are easy to twist crystal orientation and are unified into the crystal orientation of the lowest energy state, thereby eliminating dislocation caused by inconsistent crystal orientation and finally obtaining the aluminum nitride film with smooth surface and extremely low dislocation density.
Fig. 3 shows that a graphene film with uniform coverage is grown on a foreign substrate, and then plasma treatment is performed on the graphene film to increase dangling bonds on the surface of the graphene film, which corresponds to S1 and S2 in fig. 1.
Fig. 4 shows that AlN nucleation growth on plasma-treated graphene can result in dense AlN nucleation islands of high density and small size on a graphene-covered substrate.
Fig. 5 shows that the dense small-sized AlN core islands continue to grow to obtain an AlN film with completely merged surfaces, but the waviness of the surfaces is still relatively large, and a regularly arranged step flow morphology is not formed, which is equivalent to S3 in fig. 1.
Fig. 6 shows that after transferring the AlN thin film into a high-temperature annealing furnace in a nitrogen atmosphere and performing high-temperature annealing at a high temperature for one hour, an AlN thin film having a very flat surface was obtained, which corresponds to S4 in fig. 1.
FIG. 7 shows X-ray rocking curves (0002) and (9) obtained by X-ray diffraction analysis of an AlN thin film
The full width at half maximum of (a) is correspondingly narrowed after high-temperature annealing, which shows that the crystal quality after high-temperature annealing is improved no matter the AlN sample exists or does not exist in graphene.
Fig. 8 shows that the dislocation density data obtained from the analysis results of the AlN film after X-ray diffraction analysis shows that The Dislocation Density (TDD) reduction of the AlN film grown in the presence of graphene (55%) is 25% greater than that of the AlN film grown directly on the foreign substrate (30%), indicating that AlN grown on graphene has greater lattice repair capability during annealing.
FIG. 9 shows that DUV-LED prepared using the obtained AlN as a substrate has a better electroluminescence intensity than that obtained without graphene.
Therefore, it can be speculated that, for an aluminum nitride film epitaxial on a foreign substrate, graphene is used as a buffer layer to nucleate in a small size to form the film, and then high-temperature annealing treatment is carried out by using a high-temperature annealing technology.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method of growing a high quality aluminum nitride film on a foreign substrate, comprising:
s1, growing a graphene film on the foreign substrate;
s2, carrying out plasma treatment on the graphene film to form a large number of dangling bonds on the surface of the graphene film;
s3, depositing an aluminum nitride film on the surface of the graphene film by metal organic chemical vapor deposition;
and S4, annealing at high temperature to obtain the aluminum nitride film with smooth surface structure and low dislocation density.
2. The method of claim 1, wherein the plasma treatment conditions in S2 include exposure to a nitrogen atmosphere at a power of 30-100 w for a time of 30-50S.
3. The method of claim 3, wherein the plasma treatment in S2 comprises plasma treatment using a dispenser.
4. The method of claim 1, wherein the pressure of the chamber for MOCVD at S3 is 50-60 torr and the temperature is 1100-1300 ℃.
5. The method for growing a high quality aluminum nitride thin film on a foreign substrate as claimed in claim 1, wherein the high temperature annealing in S4 includes performing a high temperature annealing under a nitrogen atmosphere.
6. The method for growing a high-quality aluminum nitride thin film on a foreign substrate according to claim 1, wherein the temperature of the high temperature annealing in S4 is not lower than 1600 ℃.
7. The method for growing a high-quality aluminum nitride thin film on a foreign substrate according to claim 1, wherein the high temperature annealing in S4 is performed for 1-1.5 hours.
8. The method for growing a high-quality aluminum nitride thin film on a foreign substrate according to claim 1, wherein the method for growing the graphene thin film in S1 comprises a chemical vapor deposition method, a high temperature sublimation method.
9. The method for growing a high-quality aluminum nitride thin film on a foreign substrate according to claim 1, wherein the conditions for growing the graphene thin film in S1 include: the reactants are methane and argon, the temperature is over 1200 ℃, and the time is 3-4 hours.
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- 2020-09-27 CN CN202011036503.6A patent/CN114284397A/en active Pending
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| US20150084074A1 (en) * | 2013-09-26 | 2015-03-26 | International Business Machines Corporation | Gallium nitride material and device deposition on graphene terminated wafer and method of forming the same |
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