CN111415858A - Preparation method and application of AlN or AlGaN thin film material - Google Patents
Preparation method and application of AlN or AlGaN thin film material Download PDFInfo
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- CN111415858A CN111415858A CN202010171610.3A CN202010171610A CN111415858A CN 111415858 A CN111415858 A CN 111415858A CN 202010171610 A CN202010171610 A CN 202010171610A CN 111415858 A CN111415858 A CN 111415858A
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- 239000000463 material Substances 0.000 title claims abstract description 56
- 229910002704 AlGaN Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000010409 thin film Substances 0.000 title claims description 39
- 239000000758 substrate Substances 0.000 claims abstract description 97
- 238000010894 electron beam technology Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000002207 thermal evaporation Methods 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 58
- 229910052594 sapphire Inorganic materials 0.000 claims description 36
- 239000010980 sapphire Substances 0.000 claims description 36
- 229910052757 nitrogen Inorganic materials 0.000 claims description 29
- 238000004140 cleaning Methods 0.000 claims description 22
- 239000010408 film Substances 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000006911 nucleation Effects 0.000 claims description 5
- 238000010899 nucleation Methods 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 3
- 229910002601 GaN Inorganic materials 0.000 claims description 2
- 230000005693 optoelectronics Effects 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 7
- 230000007547 defect Effects 0.000 abstract description 3
- 238000001451 molecular beam epitaxy Methods 0.000 description 14
- 238000007664 blowing Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000005121 nitriding Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/0242—Crystalline insulating materials
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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
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
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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
- 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
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- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
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Abstract
The invention provides a preparation method of an AlN or AlGaN film material, which comprises the following steps: preparing an AlN buffer layer or a nucleating layer on a substrate by using an electron beam Al source furnace; preparing an AlN or AlGaN main epitaxial layer on the surface of the AlN buffer layer or the nucleating layer by using an electron beam Al source furnace; compared with the traditional thermal evaporation source furnace, the method for preparing the AlN or AlGaN film material can effectively improve the surface appearance of a sample under the same other growth conditions, enables the growth mode to be more easily layered growth, reduces the probability of generating new defects at the interface of the AlN film and the substrate, reduces the dislocation density of the material, improves the surface smoothness, improves the quality of the material, can further improve the performance of a deep ultraviolet light emitting and detecting device, and provides a foundation for the wide application field of military and civilian.
Description
Technical Field
The invention relates to the technical field of preparation of nitride-based materials, in particular to a preparation method and application of an AlN or AlGaN film material.
Background
In recent years, nitride materials, as representative materials of third-generation wide bandgap semiconductors, are widely applied to short-wave optoelectronic devices, ultraviolet photoelectric detection devices, high-temperature electronic devices, and high-field high-power electronic devices, and have profound effects on the fields of illumination, electronic power, and the like. At present, the device process based on GaN and a low In component GaInN material system is mature, and the growth of AlGaN materials with wider band gap and important significance In the fields of deep ultraviolet light emission detection and the like is unsatisfactory. The preparation of high-performance devices is based on the growth of high-quality materials.
Like growing high Al component AlGaN materials today, AlN templates are generally adopted as substrates, and due to the intrinsic problems of low Al atomic mobility and the like, growing high-quality AlN templates and high-quality AlN and AlGaN epitaxial films has high difficulty. In the existing method for preparing the AlN and AlGaN films by adopting a plasma-assisted molecular beam epitaxy method, a high-temperature thermal evaporation source furnace is adopted, and the prepared film material has high dislocation density and poor surface flatness. Based on this, it is necessary to improve the existing method for preparing AlN or AlGaN thin film materials.
Disclosure of Invention
In view of the above, the invention provides a preparation method of an AlN or AlGaN thin film material with small dislocation density and surface flatness.
The technical scheme of the invention is realized as follows: the invention provides a preparation method of an AlN thin film material, which comprises the following steps:
s1, preparing an AlN buffer layer or a nucleating layer on the substrate by using an electron beam Al source furnace;
s2, preparing an AlN main epitaxial layer on the surface of the AlN buffer layer or the nucleating layer by using an electron beam Al source furnace;
the process parameters for preparing the AlN buffer layer or the nucleation layer and preparing the AlN main epitaxial layer to control the electron beam Al source furnace are that the equivalent beam current generated by the electron beam Al source furnace is controlled to be 9 × 10-8-5×10-7Torr and voltage of 15-22 kV.
Based on the technical scheme, preferably, the preparation of the AlN buffer layer in S1 is realized by controlling the equivalent beam current generated by an electron beam Al source furnace to be 9 × 10 in a growth chamber-8-5×10-7The Torr and the voltage are 15-22kV, the nitrogen flow is controlled to be 0.8-1.4sccm, the substrate temperature is kept at 620-680 ℃ and the growth is carried out for 8-12min, thus obtaining the AlN buffer layer.
Further preferably, the preparation of the AlN main epitaxial layer in S2 specifically includes: under the condition of keeping the technological parameters of the electron beam Al source furnace and the nitrogen flow unchanged, the substrate temperature is increased to 820-.
The invention also provides a preparation method of the AlGaN film material, which comprises the following steps:
a1, preparing an AlN buffer layer or a nucleating layer on the substrate by using an electron beam Al source furnace;
a2, preparing an AlGaN main epitaxial layer on the surface of the AlN buffer layer or the nucleation layer by using an electron beam Al source furnace;
the process parameters for preparing the AlN buffer layer or the nucleating layer and preparing the AlGaN main epitaxial layer to control the electron beam Al source furnace are that the equivalent beam current generated by the electron beam Al source furnace is controlled to be 9 × 10-8-5×10-7Torr and voltage of 15-22 kV.
Based on the technical scheme, preferably, the preparation of the AlN buffer layer in A1 is realized by controlling the equivalent beam current generated by an electron beam Al source furnace to be 9 × 10 in a growth chamber-8-5×10-7The Torr and the voltage are 15-22kV, the nitrogen flow is controlled to be 0.8-1.4sccm, the substrate temperature is kept at 620-680 ℃ and the growth is carried out for 8-12min, thus obtaining the AlN buffer layer.
Further preferably, the preparation of the AlGaN main epitaxial layer in a2 specifically comprises the following steps: in a furnace for maintaining electron beam Al sourceUnder the condition of unchanged process parameters and nitrogen flow, the equivalent beam current generated by the thermal evaporation Ga source furnace is controlled to be 5 × 10-8-2×10-7And Torr and raising the substrate temperature to 820-.
Further preferably, before the AlN buffer layer is prepared, the substrate is further subjected to nitridation treatment, wherein the nitrogen flow rate of the nitridation treatment is 0.8-1.4sccm, the substrate temperature is 620-680 ℃, and the treatment time is 15-25 min.
Further preferably, the method further comprises performing a cleaning process on the substrate before preparing the AlN buffer layer or nucleation layer, wherein the cleaning process specifically comprises: the substrate is sequentially placed in trichloroethylene, acetone, ethanol and deionized water for ultrasonic cleaning, then the substrate is dried by using nitrogen, and is treated for 1-3h at 600-680 ℃ in an MBE pretreatment chamber.
Further preferably, the substrate includes sapphire, sapphire-based AlN, sapphire-based GaN, silicon, or silicon carbide.
The invention also provides application of the prepared AlN thin film material or AlGaN thin film material in a photoelectronic device or an ultraviolet photoelectric detector.
Compared with the prior art, the preparation method of the AlN or AlGaN film material has the following beneficial effects:
compared with the traditional thermal evaporation source furnace, the method for preparing the AlN or AlGaN film material can effectively improve the surface appearance of the film material under the same other growth conditions, enables the growth mode to be more easily layered growth, reduces the probability of generating new defects at the interface of the AlN film and the substrate, reduces the dislocation density of the material, improves the surface smoothness, improves the quality of the material, can further improve the performance of a deep ultraviolet light emitting and detecting device, and provides a foundation for the wide application field of military and civilian.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a surface SEM photograph of an AlN thin film material prepared in example 1 of the present invention;
FIG. 2 is a TEM cross-section of an AlN thin-film material prepared in example 2 of the present invention;
FIG. 3 is a surface SEM photograph of the AlN thin film material prepared in comparative example 1;
FIG. 4 is a TEM cross-sectional view of the AlN thin-film material prepared in comparative example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A preparation method of an AlN thin film material, which prepares an AlN thin film on a c-plane sapphire substrate by using a plasma-assisted molecular beam epitaxy (P-MBE) technology, comprises the following steps:
s1, cleaning the sapphire substrate, wherein the cleaning specifically comprises the following steps: sequentially placing the substrate in trichloroethylene, acetone, ethanol and deionized water, ultrasonically cleaning for 15 minutes, then blowing the sapphire substrate by using nitrogen, then placing the blown substrate into a pretreatment chamber of MBE equipment, and treating for 2 hours at 650 ℃ to remove various gases adsorbed on the surface of the substrate for later use;
s2, moving the sapphire substrate into a growth chamber, and performing nitridation treatment, wherein the nitridation treatment specifically comprises the following steps: the nitrogen source is turned on and the RF power is kept fixed at 350W, and N is controlled2The flow is 1.2sccm, the substrate temperature is 650 ℃, and the nitriding treatment time is 20 min;
s3 growing low-temperature AlN buffer layer after nitridation treatmentPreparing an AlN buffer layer by using an electron beam Al source furnace while keeping the nitrogen source parameter unchanged, wherein the equivalent beam current generated by the electron beam Al source furnace is 3.2 × 10-7Torr and voltage are 20kV, the substrate temperature is kept at 650 ℃ for 10 minutes of growth, and an AlN buffer layer is obtained; the electron beam Al source furnace bombards an Al block by using an electron beam to generate Al atoms for the growth of AlN;
and S4, raising the temperature of the substrate to 850 ℃, and continuing to grow for 2h to obtain the high-temperature AlN main epitaxial layer.
Fig. 1 is a surface SEM image of the AlN thin film material prepared in example 1, and it can be seen from fig. 1 that the entire surface of the sample is relatively flat and has good film-forming properties, and some large grains with regular hexagonal shapes can be seen.
Example 2
A preparation method of an AlN thin film material is characterized in that an AlN thin film is prepared on a sapphire-based AlN substrate by utilizing a plasma-assisted molecular beam epitaxy (P-MBE) technology, and specifically comprises the following steps:
s1, cleaning the sapphire-based AlN substrate, wherein the cleaning specifically comprises the following steps: sequentially placing the substrate in trichloroethylene, acetone, ethanol and deionized water, ultrasonically cleaning for 15 minutes, then blowing the sapphire-based AlN substrate by using nitrogen, then placing the blown substrate into a pretreatment chamber of MBE equipment, and treating for 2 hours at 650 ℃ to remove various gases adsorbed on the surface of the substrate for later use;
s2, the sapphire-based AlN substrate is moved into a growth chamber, an electron beam Al source furnace is used for preparing an AlN main epitaxial layer, and the commercial sapphire-based AlN is used as the substrate, so that the main epitaxial layer is directly prepared on the sapphire-based AlN substrate, and the specific process comprises the following steps: the nitrogen source is turned on and the RF power is kept fixed at 350W, and N is controlled2The flow rate is 1.2sccm, and the equivalent beam current generated by the electron beam Al source furnace is 3.2 × 10-7The Torr and the voltage are 20kV, and the substrate temperature is kept at 850 ℃ for growing for 2h, thus obtaining the main epitaxial layer.
FIG. 2 is a TEM cross-sectional view of the AlN thin film material prepared in example 2. from FIG. 2, it can be seen that the AlN thin film is almost integrated with the substrate, and it is difficult to see a clear boundary. No new threading dislocation is generated on the epitaxial interface, and the AlN thin film has excellent continuity.
Example 3
A preparation method of an AlGaN film material is characterized in that an AlGaN film is prepared on a c-plane sapphire substrate by utilizing a plasma-assisted molecular beam epitaxy (P-MBE) technology, and specifically comprises the following steps:
a1, cleaning the sapphire substrate, wherein the cleaning specifically comprises the following steps: sequentially placing the substrate in trichloroethylene, acetone, ethanol and deionized water, ultrasonically cleaning for 15 minutes, then blowing the sapphire substrate by using nitrogen, then placing the blown substrate into a pretreatment chamber of MBE equipment, and treating for 2 hours at 650 ℃ to remove various gases adsorbed on the surface of the substrate for later use;
a2, moving the sapphire substrate into a growth chamber, and performing nitridation treatment, wherein the nitridation treatment specifically comprises the following steps: opening a nitrogen source, keeping the radio frequency power of the nitrogen source fixed at 350W, enabling the flow of N2 to be 1.2sccm, the temperature of the substrate to be 650 ℃, and the nitriding treatment time to be 20 min;
a3, growing a low-temperature AlN buffer layer after nitridation treatment, keeping nitrogen source parameters unchanged, and preparing the AlN buffer layer by using an electron beam Al source furnace, wherein the equivalent beam current generated by the electron beam Al source furnace is 3.2 × 10-7Torr and voltage are 20kV, the substrate temperature is kept at 650 ℃ for 10 minutes of growth, and an AlN buffer layer is obtained;
a4, raising the temperature of the substrate to 850 ℃, and simultaneously controlling the equivalent beam current generated by the thermal evaporation Ga source furnace to be 8.6 × 10- 8And (5) continuing to grow for 2 hours by Torr to obtain the AlGaN main epitaxial layer.
Example 4
A preparation method of an AlGaN film material utilizes a plasma-assisted molecular beam epitaxy (P-MBE) technology to prepare an AlGaN film on a sapphire-based AlN substrate, and specifically comprises the following steps:
s1, cleaning the sapphire-based AlN substrate, wherein the cleaning specifically comprises the following steps: sequentially placing the substrate in trichloroethylene, acetone, ethanol and deionized water, ultrasonically cleaning for 15 minutes, then blowing the sapphire-based AlN substrate by using nitrogen, then placing the blown substrate into a pretreatment chamber of MBE equipment, and treating for 2 hours at 650 ℃ to remove various gases adsorbed on the surface of the substrate for later use;
s2, moving the sapphire-based AlN substrate into a growth chamber, preparing an AlGaN main epitaxial layer by using an electron beam Al source furnace, and directly preparing the main epitaxial layer on the sapphire-based AlN substrate because commercial sapphire-based AlN is adopted as the substrate, wherein the specific process comprises the steps of opening a nitrogen source, keeping the radio frequency power of the nitrogen source fixed at 350W, enabling the flow of N2 to be 1.2sccm, and enabling the equivalent beam current generated by the electron beam Al source furnace to be 3.2 × 10-7Torr and voltage are 20kV, and the equivalent beam current generated by a thermal evaporation Ga source furnace is controlled to be 8.6 × 10-8And (5) Torr, and growing for 2h while keeping the substrate temperature at 850 ℃ to obtain the AlGaN main epitaxial layer.
Comparative example 1
A preparation method of an AlN thin film material, which prepares an AlN thin film on a c-plane sapphire substrate by using a plasma-assisted molecular beam epitaxy (P-MBE) technology, comprises the following steps:
s1, cleaning the sapphire substrate, wherein the cleaning specifically comprises the following steps: sequentially placing the substrate in trichloroethylene, acetone, ethanol and deionized water, ultrasonically cleaning for 15 minutes, then blowing the sapphire substrate by using nitrogen, then placing the blown substrate into a pretreatment chamber of MBE equipment, and treating for 2 hours at 650 ℃ to remove various gases adsorbed on the surface of the substrate for later use;
s2, moving the sapphire substrate into a growth chamber, and performing nitridation treatment, wherein the nitridation treatment specifically comprises the following steps: the nitrogen source is turned on and the RF power is kept fixed at 350W, and N is controlled2The flow is 1.2sccm, the substrate temperature is 650 ℃, and the nitriding treatment time is 20 min;
s3, growing a low-temperature AlN buffer layer after nitriding treatment, keeping nitrogen source parameters unchanged, and preparing the AlN buffer layer by using a thermal evaporation Al source furnace, wherein the equivalent beam current generated by the thermal evaporation Al source furnace is 3.2 × 10-7The temperature of a Torr and a thermal evaporation Al source furnace is 1100 ℃, the temperature of a substrate is 650 ℃ and the substrate grows for 10 minutes, and an AlN buffer layer is obtained;
and S4, raising the temperature of the substrate to 850 ℃, and continuing to grow for 2h to obtain the main epitaxial layer.
Fig. 3 shows the AlN thin film material prepared in comparative example 1, and it can be seen from fig. 3 that the surface of the AlN thin film material is mainly composed of some large-sized particles, and at the same time, the particles are not all regular hexagonal, and some of them are circular, and exhibit a distinct island-like growth characteristic.
Comparative example 2
A preparation method of an AlN thin film material is characterized in that an AlN thin film is prepared on a sapphire-based AlN substrate by utilizing a plasma-assisted molecular beam epitaxy (P-MBE) technology, and specifically comprises the following steps:
s1, cleaning the sapphire-based AlN substrate, wherein the cleaning specifically comprises the following steps: sequentially placing the substrate in trichloroethylene, acetone, ethanol and deionized water, ultrasonically cleaning for 15 minutes, then blowing the sapphire-based AlN substrate by using nitrogen, then placing the blown substrate into a pretreatment chamber of MBE equipment, and treating for 2 hours at 650 ℃ to remove various gases adsorbed on the surface of the substrate for later use;
s2, the sapphire-based AlN substrate is moved into a growth chamber, an AlN main epitaxial layer is prepared by using a thermal evaporation Al source furnace, and the commercial sapphire-based AlN substrate is adopted as the substrate, so the main epitaxial layer is directly prepared on the sapphire-based AlN substrate, and the specific process comprises the following steps: the nitrogen source is turned on and the RF power is kept fixed at 350W, and N is controlled2The flow rate is 1.2sccm, and the equivalent beam current generated by the thermal evaporation Al source furnace is 3.2 × 10-7The temperature of a Torr and a thermal evaporation Al source furnace is 1100 ℃, the temperature of the substrate is kept at 850 ℃ for growing for 2h, and the main epitaxial layer is obtained.
FIG. 4 shows the AlN thin film material prepared in comparative example 2, and it can be seen from FIG. 4 that a clear boundary exists between the AlN thin film and the substrate, some new threading dislocations are generated at the epitaxial interface, and the quality of the AlN thin film is reduced relative to the substrate.
The invention solves the problems existing in the prior art by utilizing the electron beam source furnace to generate beam atoms with higher energy, AlN has higher bond energy relative to GaN, which causes that Al atoms have lower mobility on the surface of the substrate and are not beneficial to the layered growth in the epitaxial process. Besides the technical difficulty, the thermal mismatch between the epitaxial film and the substrate is further increased by simply raising the substrate temperature. Compared with the traditional thermal evaporation source furnace, the electron beam source furnace can generate beam atoms with higher kinetic energy, mainly because the maximum heating temperature of the thermal evaporation source furnace even with high temperature is about 1100 ℃, and the electron beam source furnace can easily reach 3500 ℃. And because electron beam is used for directly heating the growth raw materials in the electron beam source furnace, higher purity can be obtained compared with thermal evaporation, and for the electron beam A1 source furnace, the problem that higher preparation temperature must be kept in the thermal evaporation source furnace for preventing liquid aluminum from solidifying can be avoided, and the difficulty of maintenance is reduced.
Compared with the traditional thermal evaporation source furnace, the electron beam Al source furnace can effectively improve the surface appearance of a sample under the same growth conditions, enables the growth mode to be more easily layered growth, reduces the probability of generating new defects at the interface of the AlN film and the substrate, reduces the dislocation density of the material, improves the surface smoothness, improves the quality of the material, can further improve the performance of a deep ultraviolet light emitting and detecting device, and provides a foundation for the wide application field of military and civilian.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of an AlN thin film material is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing an AlN buffer layer or a nucleating layer on the substrate by using an electron beam Al source furnace;
s2, preparing an AlN main epitaxial layer on the surface of the AlN buffer layer or the nucleating layer by using an electron beam Al source furnace;
the process parameters for preparing the AlN buffer layer or the nucleation layer and preparing the AlN main epitaxial layer to control the electron beam Al source furnace are that the equivalent beam current generated by the electron beam Al source furnace is controlled to be 9 × 10-8-5×10-7Torr and voltage of 15-22 kV.
2. The method of claim 1The preparation method of the AlN thin film material is characterized in that the AlN buffer layer is prepared in S1, and specifically, in a growth chamber, the equivalent beam current generated by an electron beam Al source furnace is controlled to be 9 × 10-8-5×10-7The Torr and the voltage are 15-22kV, the nitrogen flow is controlled to be 0.8-1.4sccm, the substrate temperature is kept at 620-680 ℃ and the growth is carried out for 8-12min, thus obtaining the AlN buffer layer.
3. The method for preparing an AlN film material according to claim 2, wherein: the preparation of the AlN main epitaxial layer in the S2 specifically comprises the following steps: under the condition of keeping the technological parameters of the electron beam Al source furnace and the nitrogen flow unchanged, the substrate temperature is increased to 820-.
4. A preparation method of AlGaN film material is characterized by comprising the following steps: the method comprises the following steps:
a1, preparing an AlN buffer layer or a nucleating layer on the substrate by using an electron beam Al source furnace;
a2, preparing an AlGaN main epitaxial layer on the surface of the AlN buffer layer or the nucleation layer by using an electron beam Al source furnace;
the process parameters for preparing the AlN buffer layer or the nucleating layer and preparing the AlGaN main epitaxial layer to control the electron beam Al source furnace are that the equivalent beam current generated by the electron beam Al source furnace is controlled to be 9 × 10-8-5×10-7Torr and voltage of 15-22 kV.
5. The method according to claim 4, wherein the step of preparing the AlN buffer layer in A1 is carried out by controlling the equivalent beam current generated by an electron beam Al source furnace to 9 × 10 in a growth chamber-8-5×10-7The Torr and the voltage are 15-22kV, the nitrogen flow is controlled to be 0.8-1.4sccm, the substrate temperature is kept at 620-680 ℃ and the growth is carried out for 8-12min, thus obtaining the AlN buffer layer.
6. The method of manufacturing an AlGaN thin film material according to claim 5, wherein: the preparation of the AlGaN main epitaxial layer in a2 specifically comprises the following steps: under the condition of keeping the technological parameters of the electron beam Al source furnace and the nitrogen flow unchanged,controlling the equivalent beam current generated by the thermal evaporation Ga source furnace to be 5 × 10-8-2×10-7And Torr and raising the substrate temperature to 820-.
7. The method for producing an AlN thin film material according to claim 2 or the method for producing an AlGaN thin film material according to claim 5, wherein: before preparing the AlN buffer layer, the substrate is further subjected to nitridation treatment, wherein the nitrogen flow rate of the nitridation treatment is 0.8-1.4sccm, the substrate temperature is 620-680 ℃, and the treatment time is 15-25 min.
8. The method for producing an AlN thin film material according to claim 1 or the method for producing an AlGaN thin film material according to claim 4, wherein: the method also comprises the following step of cleaning the substrate before preparing the AlN buffer layer or the AlN nucleating layer, wherein the cleaning process specifically comprises the following steps: the substrate is sequentially placed in trichloroethylene, acetone, ethanol and deionized water for ultrasonic cleaning, then the substrate is dried by using nitrogen, and is treated for 1-3h at 600-680 ℃ in an MBE pretreatment chamber.
9. The method for producing an AlN thin film material according to claim 1 or the method for producing an AlGaN thin film material according to claim 4, wherein: the substrate comprises sapphire, sapphire-based AlN, sapphire-based GaN, silicon or silicon carbide.
10. An application of the AlN thin film material or the AlGaN thin film material prepared by the preparation method of claim 1 or 4 in an optoelectronic device or an ultraviolet photoelectric detection device.
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