CN112151645A - Preparation of large-angle oblique-cutting sapphire substrate AlN, light-emitting diode and preparation method thereof - Google Patents
Preparation of large-angle oblique-cutting sapphire substrate AlN, light-emitting diode and preparation method thereof Download PDFInfo
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- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 179
- 239000010980 sapphire Substances 0.000 title claims abstract description 179
- 239000000758 substrate Substances 0.000 title claims abstract description 179
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 238000005520 cutting process Methods 0.000 title abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 58
- 229910002704 AlGaN Inorganic materials 0.000 claims description 71
- 238000000034 method Methods 0.000 claims description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
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- 239000002184 metal Substances 0.000 claims description 6
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- 238000009616 inductively coupled plasma Methods 0.000 claims description 4
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- 239000010409 thin film Substances 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 description 23
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0075—Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/04—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table
- H01L33/32—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen
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Abstract
The invention discloses a preparation method of a large-angle oblique cutting sapphire substrate AlN, a light emitting diode and a preparation method thereof, wherein the preparation method of the large-angle oblique cutting sapphire substrate AlN comprises the following steps: selecting a large-angle oblique-cutting sapphire substrate and a conventional sapphire substrate; growing AlN layers on the large-angle beveling sapphire substrate and the conventional sapphire substrate respectively to obtain a large-angle beveling sapphire substrate AlN epitaxial layer and a conventional sapphire substrate AlN epitaxial layer; attaching the AlN growth surface of the AlN epitaxial layer of the large-angle beveling sapphire substrate with the AlN growth surface of the AlN epitaxial layer of the conventional sapphire substrate, and carrying out high-temperature annealing; and repeatedly growing an AlN layer on the AlN epitaxial layer of the large-angle beveling sapphire substrate after high-temperature annealing, and carrying out high-temperature annealing until the AlN layer on the AlN epitaxial layer of the large-angle beveling sapphire substrate after high-temperature annealing reaches a preset thickness. According to the invention, the high-quality AlN thin film is prepared on the large-angle beveling sapphire substrate by annealing the large-angle beveling sapphire substrate after the AlN thin film is grown.
Description
Technical Field
The invention belongs to the technical field of wide bandgap semiconductors, and particularly relates to a preparation method of a large-angle beveling sapphire substrate AlN, a preparation method of a light emitting diode and the light emitting diode.
Background
In the prior art, the AlGaN-based solid deep ultraviolet light source has the advantages of environmental protection, long service life and the like, and is a key technology for replacing the traditional mercury lamp. AlGaN as a wide bandgap semiconductor has been proven to be one of the ideal choices for clean and environmentally friendly Deep Ultraviolet (DUV) light sources sought by people.
Compared with the mature technology of blue light LEDs based on InGaN base, the external quantum efficiency of Deep ultraviolet light emitting diodes (DUV-LEDs) based on AlGaN is lower than 10% in most cases. The large-angle beveled substrate can increase the overlap of electron wave functions and enhance carrier localization, and is very necessary for improving the radiation recombination efficiency and the internal quantum efficiency. The mesa density can be effectively reduced by increasing the substrate beveling angle, and the atoms can be effectively merged into the step position under the condition of smaller migration length. Epitaxial structures based on large angle beveling substrates have many advantages, and AlN films have been prepared on conventional C-plane sapphire substrates by a number of methods, including continuous high temperature growth based on metal organic Vapor Phase growth, Hydride Vapor Phase Epitaxy (HVPE for short), and molecular beam Epitaxy.
However, the most critical problem is still the problem of AlN epitaxial growth, and the above-mentioned solutions do not solve the problem of poor dislocation density and poor surface morphology of the AlN structure epitaxially grown on the large-angle-bias sapphire. High temperature and high pressure equipment and accurate flow control systems are required for AlN production. The crystal quality prepared by the current expensive commercial High Temperature Metal Organic Chemical Vapor Deposition (HT-MOCVD) has a larger promotion space, the lattice constant difference between the AlN material and the sapphire substrate is huge, and larger thermal mismatch exists, so that the AlN surface is easy to crack, and the development of deep ultraviolet devices on large-angle beveling sapphire substrates is greatly limited.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a large-angle beveling sapphire substrate AlN, a preparation method of a light-emitting diode and the light-emitting diode.
One embodiment of the invention provides a preparation method of a large-angle beveling sapphire substrate AlN, which comprises the following steps:
selecting a large-angle beveling sapphire substrate and a conventional sapphire substrate;
growing an AlN layer on the large-angle beveled sapphire substrate to obtain a large-angle beveled sapphire substrate AlN epitaxial layer, and growing an AlN layer on the conventional sapphire substrate to obtain a conventional sapphire substrate AlN epitaxial layer;
the AlN growth surface of the large-angle beveling sapphire substrate AlN epitaxial layer is attached to the AlN growth surface of the conventional sapphire substrate AlN epitaxial layer, the high-temperature annealing is carried out in a high-temperature annealing furnace, and the large-angle beveling sapphire substrate AlN epitaxial layer and the conventional sapphire substrate AlN epitaxial layer after the high-temperature annealing are peeled off;
and repeatedly growing an AlN layer on the high-angle beveling sapphire substrate AlN epitaxial layer after high-temperature annealing, and carrying out high-temperature annealing treatment until the AlN layer on the high-angle beveling sapphire substrate AlN epitaxial layer after high-temperature annealing reaches a preset thickness so as to finish the preparation of the high-angle beveling sapphire substrate AlN.
In one embodiment of the invention, the chamfering direction of the large-angle chamfering sapphire substrate is that a c surface is deviated to an a surface, and the chamfering angle range is 0.2-6 degrees;
in one embodiment of the invention, the AlN layer grown on the large-angle beveling sapphire substrate has the thickness of 200 nm-400 nm.
In one embodiment of the invention, the AlN layer grown on the conventional sapphire substrate has a thickness of 200nm to 300 nm.
In an embodiment of the invention, the step of attaching the AlN growth surface of the large-angle miscut sapphire substrate AlN epitaxial layer to the AlN growth surface of the conventional sapphire substrate AlN epitaxial layer, and the step of placing the conventional sapphire substrate AlN epitaxial layer in a high-temperature annealing furnace for high-temperature annealing includes:
and (2) vertically attaching the AlN growth surface of the AlN epitaxial layer of the large-angle beveling sapphire substrate with the AlN growth surface of the AlN epitaxial layer of the conventional sapphire substrate, and placing the bonded layer in a high-temperature annealing furnace, wherein the AlN growth surface of the AlN epitaxial layer of the large-angle beveling sapphire substrate is arranged below, the AlN growth surface of the AlN epitaxial layer of the conventional sapphire substrate is arranged above, and the process conditions are as follows: introducing nitrogen and argon into the high-temperature annealing furnace, wherein the volume ratio of the introduced nitrogen to the introduced argon is 3:1, and the pressure in the high-temperature annealing furnace is kept at 0.03-0.6 atmospheric pressure; the temperature of the high-temperature annealing furnace is raised to 1600-1750 ℃, and the high-temperature annealing treatment is carried out after the heat preservation for 1-3 h; and after the high-temperature annealing is finished, quickly cooling the high-temperature annealing furnace to room temperature.
In one embodiment of the invention, the time for rapidly cooling the high-temperature annealing furnace to the room temperature is controlled to be 0.5 h-1.5 h.
In one embodiment of the invention, the AlN layer of the AlN epitaxial layer of the large-angle beveling sapphire substrate is preset to be 0.2-5 μm thick.
Another embodiment of the present invention provides a method for manufacturing a light emitting diode, including:
preparing a large-angle beveling sapphire substrate AlN epitaxial layer by any one of the above preparation methods of the large-angle beveling sapphire substrate AlN, wherein the AlN layer of the large-angle beveling sapphire substrate AlN epitaxial layer has a preset thickness;
growing an AlN homogeneous epitaxial layer on the AlN growth surface of the large-angle beveling sapphire substrate AlN epitaxial layer;
growing an n-type AlGaN layer on the AlN homoepitaxial layer;
growing an AlGaN/AlN multi-quantum well layer on the n-type AlGaN layer;
growing an AlGaN electron barrier layer on the AlGaN/AlN multi-quantum well layer;
growing a p-type AlGaN layer on the AlGaN electron blocking layer;
and etching part of the p-type AlGaN layer to an n-type AlGaN layer by adopting an inductively coupled plasma etching process to form an n-type AlGaN table top, respectively depositing an n-type electrode on the n-type AlGaN table top by adopting a metal sputtering method, and depositing a p-type electrode on the other part of the p-type AlGaN layer to finish the preparation of the light-emitting diode.
In one embodiment of the invention, the chamfering direction of the large-angle chamfering sapphire substrate is that the c plane deviates to the a plane, and the chamfering angle ranges from 0.2 degrees to 6 degrees.
The invention further provides a light-emitting diode prepared by the preparation method of any one of the light-emitting diodes.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the large-angle beveling sapphire substrate AlN, the high-quality AlN thin film is prepared on the large-angle beveling sapphire substrate by annealing the large-angle beveling sapphire substrate after the AlN thin film is grown, so that the large-angle beveling sapphire/AlN which is low in dislocation density, smooth in surface and good in uniformity is obtained as a template, and the problems of high AlN dislocation density, poor surface roughness and the like in the existing AlN growth technology are effectively solved.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a large-angle beveling sapphire substrate AlN according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an ultraviolet transmission spectrum test provided by an embodiment of the present invention;
FIG. 3 is a graph showing the comparison of the test results of the rocking curves of the AlN epitaxial layer prepared by the present invention and the AlN epitaxial layer prepared by the conventional PVD in the X-ray diffraction (002) plane;
FIG. 4 is a graph showing the comparison of the swing curves of the AlN epitaxial layer prepared by the present invention and the AlN epitaxial layer prepared by the conventional PVD in the X-ray diffraction (102) plane;
fig. 5 is a schematic flow chart of a method for manufacturing a light emitting diode according to an embodiment of the present invention;
fig. 6 is a schematic diagram showing a comparison of test results of a rocking curve of an X-ray diffraction (002) plane of an n-type AlGaN layer regrown on a high-temperature annealed AlN layer in a method for manufacturing a light emitting diode according to an embodiment of the present invention;
fig. 7 is a schematic diagram comparing the test results of the rocking curve of the n-type AlGaN layer regrown on the high temperature annealed AlN layer in the method for manufacturing a light emitting diode according to the embodiment of the present invention on the X-ray diffraction (102) plane;
fig. 8 is a schematic structural diagram of a light emitting diode according to an embodiment of the present invention.
Description of reference numerals:
1-chamfering the AlN epitaxial layer of the sapphire substrate at a large angle; 2-AlN homoepitaxial layer; a 3-n type AlGaN layer; a 4-AlGaN/AlN multi-quantum well layer; 5-AlGaN electron blocking layer; a 6-p type AlGaN layer; a 7-n electrode; 8-p electrode.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example one
In order to solve the problem that the dislocation density and the surface appearance of the AlN structure epitaxially grown on the large-angle miscut sapphire substrate are deteriorated, please refer to fig. 1, where fig. 1 is a schematic flow chart of a method for preparing the large-angle miscut sapphire substrate AlN according to an embodiment of the present invention. The embodiment provides a preparation method of a large-angle beveling sapphire substrate AlN, which comprises the following steps:
step 1, selecting a large-angle beveling sapphire substrate and a conventional sapphire substrate.
Specifically, the present embodiment selects a large-angle bias sapphire substrate and a conventional sapphire substrate, and respectively pre-processes the large-angle bias sapphire substrate and the conventional sapphire substrate, including: the method comprises the steps of sequentially carrying out ultrasonic cleaning on a large-angle oblique cutting sapphire substrate and a conventional sapphire substrate by acetone, dilute hydrochloric acid and deionized water, then placing the sapphire substrate and the conventional sapphire substrate in a Physical Vapor Deposition (PVD) device reaction chamber, and reducing the vacuum degree of the reaction chamber to 1 × 10-2And (3) introducing hydrogen into the reaction chamber, heating the large-angle beveled sapphire substrate and the conventional sapphire substrate to the temperature of 950-1100 ℃ under the condition that the pressure of the reaction chamber of the PVD device is 200Torr, and keeping the temperature for 10min to finish the heat treatment of the large-angle beveled sapphire substrate and the conventional sapphire substrate.
Preferably, the chamfering direction of the large-angle chamfering sapphire substrate is that the c surface deviates to the a surface, and the chamfering angle range is 0.2-6 degrees.
And 2, growing an AlN layer on the large-angle beveled sapphire substrate to obtain a large-angle beveled sapphire substrate AlN epitaxial layer, and growing an AlN layer on the conventional sapphire substrate to obtain a conventional sapphire substrate AlN epitaxial layer.
Specifically, in the embodiment, the reaction chamber atmosphere of the PVD device is replaced by high-purity nitrogen (the nitrogen content is 99.999%), the distances between the large-angle beveled sapphire substrate and the target are respectively adjusted to 4-6 cm, the temperature of the large-angle beveled sapphire substrate and the temperature of the conventional sapphire substrate are kept at 620-700 ℃, the radio frequency power is adjusted to 710-750W by using a radio frequency magnetron sputtering method, an AlN layer is physically sputtered and grown on the large-angle beveled sapphire substrate to obtain a large-angle beveled sapphire substrate AlN epitaxial layer, and an AlN layer is physically sputtered and grown on the conventional sapphire substrate to obtain a conventional sapphire substrate AlN epitaxial layer. The AlN layer grown on the large-angle beveling sapphire substrate and the AlN layer grown on the conventional sapphire substrate are both unintentionally doped AlN layers; the physical sputtering growth of the AlN layer on the conventional sapphire substrate is specifically the physical sputtering growth of the AlN layer on the c-plane of the conventional sapphire substrate.
Preferably, the thickness of the AlN layer grown on the large-angle beveling sapphire substrate is 200 nm-400 nm, and the thickness of the AlN layer grown on the conventional sapphire substrate is 200 nm-300 nm.
And 3, attaching the AlN growth surface of the large-angle beveling sapphire substrate AlN epitaxial layer with the AlN growth surface of the conventional sapphire substrate AlN epitaxial layer, placing the bonded sapphire substrate AlN epitaxial layer in a high-temperature annealing furnace for high-temperature annealing, and stripping the large-angle beveling sapphire substrate AlN epitaxial layer and the conventional sapphire substrate AlN epitaxial layer after the high-temperature annealing is finished.
Specifically, in this embodiment, the AlN growth surface of the large-angle miscut sapphire substrate AlN epitaxial layer is vertically bonded to the AlN growth surface of the conventional sapphire substrate AlN epitaxial layer, and the AlN epitaxial layer is placed in a high-temperature annealing furnace while keeping the orientation of the AlN epitaxial layer consistent, wherein the AlN growth surface of the large-angle miscut sapphire substrate AlN epitaxial layer is below, the AlN growth surface of the conventional sapphire substrate AlN epitaxial layer is above, and the process conditions are as follows: introducing nitrogen and argon into the high-temperature annealing furnace, wherein the volume ratio of the introduced nitrogen to the introduced argon is 3:1, and the pressure in the high-temperature annealing furnace is kept at 0.03-0.6 atmospheric pressure; the temperature of the high-temperature annealing furnace is raised to 1600-1750 ℃, and the high-temperature annealing treatment is carried out after the heat preservation for 1-3 h; and after the high-temperature annealing is finished, quickly cooling the high-temperature annealing furnace to room temperature. Preferably, the time for rapidly cooling the high-temperature annealing furnace to the room temperature is controlled to be 0.5 h-1.5 h.
And stripping the high-angle beveling sapphire substrate AlN epitaxial layer subjected to high-temperature annealing and cooling from the top and the bottom, and separating the high-angle beveling sapphire substrate AlN epitaxial layer from the c-plane sapphire AlN epitaxial layer, and respectively ensuring that the AlN growth surface of the high-angle beveling sapphire substrate AlN epitaxial layer and the AlN growth surface of the conventional sapphire substrate AlN epitaxial layer face upwards for subsequent reutilization.
And 4, repeatedly growing an AlN layer on the high-temperature annealed high-angle beveled sapphire substrate AlN epitaxial layer, and carrying out high-temperature annealing treatment until the AlN layer on the high-temperature annealed high-angle beveled sapphire substrate AlN epitaxial layer reaches a preset thickness so as to finish the preparation of the high-angle beveled sapphire substrate AlN.
Specifically, in this embodiment, the large-angle beveling sapphire substrate AlN epitaxial layer obtained in the step 3 is placed in a PVD device to re-sputter an AlN layer, and subjected to high-temperature annealing treatment in a high-temperature annealing furnace, and the processes in the steps 2 and 3 are repeated to obtain a high-quality large-angle beveling sapphire substrate AlN epitaxial layer with a preset thickness. And 3, completing AlN layer sputtering and high-temperature annealing each time by adopting the annealing parameters in the step 3 until the thickness of the large-angle beveling sapphire substrate AlN epitaxial layer reaches the preset thickness.
Preferably, the AlN layer of the AlN epitaxial layer of the sapphire substrate beveled at a large angle is preset to be 0.2-5 μm thick.
The effect of the method for preparing the large-angle beveling sapphire substrate AlN provided in this embodiment can be further illustrated by the following test results:
1. and (3) testing conditions are as follows:
selecting a sapphire substrate with a c surface inclined to an a surface and obliquely cutting by 4 degrees to form an 800nm AlN epitaxial layer at the room temperature of 25 ℃ in a nitrogen atmosphere environment.
2. The test contents are as follows:
test 1, please refer to fig. 2, fig. 2 is a schematic diagram of an ultraviolet transmission spectrum test provided by an embodiment of the present invention, in fig. 2, the abscissa is the unit of laser incident wavelength of the ultraviolet transmission spectrum in nm, and the ordinate is the light transmittance T of fig. 2, in this embodiment, an 800nm AlN epitaxial layer on a sapphire substrate with a c-plane inclined to a-plane and a 4 ° chamfered angle is selected for an ultraviolet transmission spectrum test, and it can be observed from fig. 2 that the 800nm AlN epitaxial layer on the sapphire substrate with a c-plane inclined to a-plane and a 4 ° chamfered angle prepared by the preparation method of this embodiment has accurate thickness control, smooth spectrum curve, and good deep ultraviolet light transmittance near 280 nm.
In summary, the preparation method of the large-angle beveling sapphire substrate AlN provided by the embodiment realizes high-quality growth of the large-angle beveling sapphire substrate AlN epitaxial layer by adjusting annealing process parameters after the AlN film is physically grown, so that the large-angle beveling sapphire/AlN with low dislocation density, smooth surface and good uniformity is obtained as a template, growth of AlGaN related devices is performed based on the template, and the problems of high AlN dislocation density, poor surface roughness and the like in the existing AlN growth technology are effectively overcome; meanwhile, the preparation method of the large-angle beveling sapphire substrate AlN is still an epitaxial technology, can be prepared only by adjusting annealing parameters, has no special requirements on growth equipment, and is simple to apply and low in cost.
Example two
On the basis of the first embodiment, please refer to fig. 5, and fig. 5 is a schematic flow chart of a method for manufacturing a light emitting diode according to an embodiment of the present invention. The embodiment provides a method for preparing a light-emitting diode, which comprises the following steps:
step 1, preparing a large-angle beveling sapphire substrate AlN epitaxial layer.
Specifically, in this embodiment, the large-angle oblique sapphire substrate AlN epitaxial layer is prepared by the method for preparing the large-angle oblique sapphire substrate AlN described in the first embodiment, and the preparation process and the technical effects of the large-angle oblique sapphire substrate AlN epitaxial layer are not repeated herein. The thickness of the large-angle beveling sapphire substrate AlN epitaxial layer is a preset thickness.
Preferably, the chamfering direction of the large-angle chamfering sapphire substrate is that the c plane deviates from the a plane, and the chamfering angle ranges from 0.2 degrees to 6 degrees.
Preferably, the AlN layer of the AlN epitaxial layer of the sapphire substrate beveled at a large angle is preset to be 0.2-5 μm thick.
And 2, growing an AlN homogeneous epitaxial layer on the AlN growth surface of the sapphire substrate AlN epitaxial layer obliquely cut at a large angle.
Specifically, in this embodiment, the c-plane obliquely-cut sapphire substrate AlN epitaxial layer with a c-plane biased to the a-plane after high temperature annealing is placed in a Metal-Organic Chemical vapor Deposition (MOCVD) device, the temperature of a reaction chamber of the MOCVD device is raised to 1120-1350 ℃, the pressure of the reaction chamber is adjusted to 85mbar, TMAl and ammonia gas are introduced, the v/iii molar ratio is maintained at 435, and an AlN homoepitaxial layer with a thickness of 0.5 μm-1 μm is grown.
And 3, growing an n-type AlGaN layer on the AlN homoepitaxial layer.
Specifically, in this example, three gases, that is, ammonia gas at a flow rate of 995sccm, a gallium source at a flow rate of 49sccm, and an aluminum source at a flow rate of 52sccm, were simultaneously introduced into an AlN homoepitaxial layer by an MOCVD process at a reaction chamber temperature of 1085 ℃, and an n-type AlGaN layer having a thickness of 1.5 μm to 2.5 μm was grown under a condition in which a pressure was maintained at 30 Torr. Wherein, Si doping can be carried out in the growth n-type AlGaN layer, and the doping concentration of Si is 5 multiplied by 1018cm-3。
And 4, growing an AlGaN/AlN multi-quantum well layer on the n-type AlGaN layer.
Specifically, in this embodiment, an MOCVD process is performed on the n-type AlGaN layer, the LED active region growth is completed at 1020 ℃ and 1120 ℃ respectively in a nitrogen atmosphere, and the growth is repeated for 8 cycles under the above conditions to obtain an AlGaN/AlN quantum well barrier with a thickness of 110nm to 150 nm.
And 5, growing an AlGaN electron barrier layer on the AlGaN/AlN multi-quantum well layer.
Specifically, in the embodiment, the temperature of the nitrogen atmosphere in the reaction chamber is kept to be increased to 1180 ℃, and the AlGaN electron blocking layer with the thickness of 35nm to 45nm is grown by adopting the MOCVD process.
And 6, growing a p-type AlGaN layer on the AlGaN electron blocking layer.
Specifically, in this embodiment, an MOCVD process is employed on the AlGaN electron blocking layer, the reaction chamber is replaced with a hydrogen atmosphere, the temperature of the reaction chamber is raised to 985 ℃, the pressure of the reaction chamber is maintained at 135Torr, ammonia gas with a flow rate of 1175sccm, a gallium source with a flow rate of 38sccm, an aluminum source with a flow rate of 195sccm and a magnesium source with a flow rate of 19sccm are introduced into the reaction chamber, a p-type AlGaN layer with a thickness of 100nm to 220nm is grown, and then the temperature of the reaction chamber is maintained at 880 ℃ for 10min to activate carriers. Wherein, Mg doping can be carried out in the growing p-type AlGaN layer, and the Mg doping concentration is 1 multiplied by 1019cm-3。
And 7, etching part of the p-type AlGaN layer to the n-type AlGaN layer by adopting an inductively coupled plasma etching process to form an n-type AlGaN table top, respectively depositing an n-type electrode on the n-type AlGaN table top by adopting a metal sputtering method, and depositing a p-type electrode on the other part of the p-type AlGaN layer to finish the preparation of the light-emitting diode.
Specifically, in the embodiment, an inductively coupled plasma etching method is adopted to partially etch a p-type AlGaN layer from the top, and the p-type AlGaN layer is etched until the n-type AlGaN layer forms an n-type AlGaN mesa, electrodes are respectively deposited on the n-type AlGaN mesa and the p-type AlGaN layer which is not etched, specifically, a metal sputtering method is adopted to deposit an n-type electrode on the n-type AlGaN mesa, and a p-type electrode is deposited on the p-type AlGaN layer, so as to complete the fabrication of the light emitting diode on the sapphire substrate AlN epitaxial layer template based on large-angle beveling.
It should be noted that the AlN epitaxial layer of the large-angle miscut sapphire substrate prepared in step 1 is not limited to be prepared by a PVD apparatus, and for example, the AlN epitaxial layer may also be prepared by a similar process using the MOCVD apparatus of this embodiment.
The effect of the method for manufacturing a light emitting diode according to the present embodiment can be further illustrated by the following test results:
1. and (3) testing conditions are as follows:
selecting a sapphire substrate with a c surface inclined to an a surface and obliquely cutting by 4 degrees to form an 800nm AlN epitaxial layer at the room temperature of 25 ℃ in a nitrogen atmosphere environment.
2. The test contents are as follows:
test 1, please refer to fig. 6, fig. 6 is a comparison diagram of test results of a rocking curve of an n-type AlGaN layer regrown on a high-temperature annealed AlN layer in a manufacturing method of a light emitting diode according to an embodiment of the present invention on an X-ray diffraction (002) plane, where the abscissa in fig. 6 is Omega angle unit arcsec, and the ordinate in fig. 6 is peak intensity after normalization processing, in this embodiment, a rocking curve of an X-ray diffraction (002) plane of an n-type AlGaN layer is tested, and it can be observed from fig. 6 that a half-height width of the rocking curve of the n-type AlGaN thin film (002) plane prepared by the manufacturing method in this embodiment is only 124arcsec, which is far lower than 809arcsec prepared by a conventional MOCVD method. The crystal quality is obviously improved, and the density of screw dislocation is obviously reduced.
In summary, the preparation method of the light emitting diode provided by the embodiment has good compatibility with the existing MOCVD-based LED preparation process, and the support technology is used together, the large-angle miscut sapphire substrate/AlN template prepared by the method of the embodiment can be used as a substrate to grow an AlGaN light emitting layer in application, the AlGaN light emitting layer emits deep ultraviolet light under the action of current, the quantum efficiency in the deep ultraviolet band LED can be remarkably improved while the quality of an Al component AlGaN material is remarkably improved, and the problem that the development of deep ultraviolet devices on the large-angle miscut sapphire substrate is limited is solved.
The method for manufacturing the light emitting diode provided in this embodiment may be implemented in the embodiment of the method for manufacturing the large-angle beveling sapphire substrate AlN, which is similar in implementation principle and technical effect and is not described herein again.
EXAMPLE III
On the basis of the second embodiment, please refer to fig. 8, and fig. 8 is a schematic structural diagram of a light emitting diode according to an embodiment of the present invention. The embodiment provides a light emitting diode, the structure of which comprises from bottom to top in sequence: the LED is prepared and formed by the LED preparation method in the second embodiment, wherein the large-angle beveling sapphire substrate AlN epitaxial layer 1 is prepared and formed by the large-angle beveling sapphire substrate AlN preparation method in the first embodiment.
The light emitting diode provided in this embodiment may implement the embodiments of the method for preparing a large-angle beveling sapphire substrate AlN and the embodiments of the method for preparing a light emitting diode described in the above first embodiment and second embodiment, and the implementation principle and technical effects are similar, and are not described herein again.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (10)
1. A preparation method of a large-angle beveling sapphire substrate AlN is characterized by comprising the following steps:
selecting a large-angle beveling sapphire substrate and a conventional sapphire substrate;
growing an AlN layer on the large-angle beveled sapphire substrate to obtain a large-angle beveled sapphire substrate AlN epitaxial layer, and growing an AlN layer on the conventional sapphire substrate to obtain a conventional sapphire substrate AlN epitaxial layer;
the AlN growth surface of the large-angle beveling sapphire substrate AlN epitaxial layer is attached to the AlN growth surface of the conventional sapphire substrate AlN epitaxial layer, the high-temperature annealing is carried out in a high-temperature annealing furnace, and the large-angle beveling sapphire substrate AlN epitaxial layer and the conventional sapphire substrate AlN epitaxial layer after the high-temperature annealing are peeled off;
and repeatedly growing an AlN layer on the high-angle beveling sapphire substrate AlN epitaxial layer after high-temperature annealing, and carrying out high-temperature annealing treatment until the AlN layer on the high-angle beveling sapphire substrate AlN epitaxial layer after high-temperature annealing reaches a preset thickness so as to finish the preparation of the high-angle beveling sapphire substrate AlN.
2. The method for preparing the large-angle beveled sapphire substrate AlN according to claim 1, wherein the beveling direction of the large-angle beveled sapphire substrate is that the c plane is deviated to the a plane, and the beveling angle ranges from 0.2 to 6 degrees.
3. The preparation method of the large-angle beveling sapphire substrate AlN according to claim 1, characterized in that the thickness of the AlN layer grown on the large-angle beveling sapphire substrate is 200 nm-400 nm.
4. The method for preparing the large-angle beveling sapphire substrate AlN according to claim 1, wherein the thickness of the AlN layer grown on the conventional sapphire substrate is 200 nm-300 nm.
5. The preparation method of the large-angle beveling sapphire substrate AlN according to claim 1, wherein the step of attaching the AlN growth face of the large-angle beveling sapphire substrate AlN epitaxial layer to the AlN growth face of the conventional sapphire substrate AlN epitaxial layer and placing the attached AlN growth face in a high-temperature annealing furnace for high-temperature annealing comprises the steps of:
and (2) vertically attaching the AlN growth surface of the AlN epitaxial layer of the large-angle beveling sapphire substrate with the AlN growth surface of the AlN epitaxial layer of the conventional sapphire substrate, and placing the bonded layer in a high-temperature annealing furnace, wherein the AlN growth surface of the AlN epitaxial layer of the large-angle beveling sapphire substrate is arranged below, the AlN growth surface of the AlN epitaxial layer of the conventional sapphire substrate is arranged above, and the process conditions are as follows: introducing nitrogen and argon into the high-temperature annealing furnace, wherein the volume ratio of the introduced nitrogen to the introduced argon is 3:1, and the pressure in the high-temperature annealing furnace is kept at 0.03-0.6 atmospheric pressure; the temperature of the high-temperature annealing furnace is raised to 1600-1750 ℃, and the high-temperature annealing treatment is carried out after the heat preservation for 1-3 h; and after the high-temperature annealing is finished, quickly cooling the high-temperature annealing furnace to room temperature.
6. The preparation method of the large-angle beveling sapphire substrate AlN according to claim 5, characterized in that the time for rapidly cooling the high-temperature annealing furnace to room temperature is controlled to be 0.5 h-1.5 h.
7. The preparation method of the large-angle beveling sapphire substrate AlN according to claim 1, characterized in that the AlN layer of the AlN epitaxial layer of the large-angle beveling sapphire substrate is preset to be 0.2-5 μm thick.
8. A method for manufacturing a light emitting diode, comprising:
preparing a large-angle beveling sapphire substrate AlN epitaxial layer by the large-angle beveling sapphire substrate AlN preparation method according to any one of claims 1 to 7, wherein the AlN layer of the large-angle beveling sapphire substrate AlN epitaxial layer has a preset thickness;
growing an AlN homogeneous epitaxial layer on the AlN growth surface of the large-angle beveling sapphire substrate AlN epitaxial layer;
growing an n-type AlGaN layer on the AlN homoepitaxial layer;
growing an AlGaN/AlN multi-quantum well layer on the n-type AlGaN layer;
growing an AlGaN electron barrier layer on the AlGaN/AlN multi-quantum well layer;
growing a p-type AlGaN layer on the AlGaN electron blocking layer;
and etching part of the p-type AlGaN layer to an n-type AlGaN layer by adopting an inductively coupled plasma etching process to form an n-type AlGaN table top, respectively depositing an n-type electrode on the n-type AlGaN table top by adopting a metal sputtering method, and depositing a p-type electrode on the other part of the p-type AlGaN layer to finish the preparation of the light-emitting diode.
9. The method of claim 8, wherein the chamfering direction of the large-angle chamfered sapphire substrate is that the c plane is deviated to the a plane, and the chamfer angle ranges from 0.2 ° to 6 °.
10. A light-emitting diode, characterized in that, the light-emitting diode is prepared by the method of any one of claims 8 to 9.
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