CN115101633A - InGaN-based optoelectronic device and preparation method thereof - Google Patents
InGaN-based optoelectronic device and preparation method thereof Download PDFInfo
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- 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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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- 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
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02455—Group 13/15 materials
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- 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
- H01L21/02436—Intermediate layers between substrates and deposited layers
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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Abstract
The invention relates to an InGaN-based optoelectronic device and a preparation method thereof. The preparation method of the InGaN-based optoelectronic device comprises the following steps: forming an AlN transition layer on the crystal substrate, wherein the AlN transition layer consists of a plurality of first three-dimensional growth islands; epitaxially growing a GaN transition layer on the AlN transition layer, wherein the GaN transition layer consists of a plurality of second three-dimensional growth small islands, and the second three-dimensional growth small islands in the GaN transition layer are the continuation of the first three-dimensional growth small islands in the AlN transition layer to obtain a composite substrate of the InGaN-based optoelectronic device; epitaxially growing a nitride conversion layer on a composite substrate of the InGaN-based optoelectronic device in a two-dimensional epitaxial mode; and forming other device structure layers of the InGaN-based optoelectronic device on the nitride conversion layer to obtain the InGaN-based optoelectronic device. The preparation method can improve the incorporation efficiency of the In component In the InGaN-based optoelectronic device. In addition, the invention also relates to an InGaN-based optoelectronic device prepared by the preparation method of the InGaN-based optoelectronic device.
Description
Technical Field
The invention relates to the technical field of optoelectronic devices, in particular to an InGaN-based optoelectronic device and a preparation method thereof.
Background
The wavelength range corresponding to the InGaN material is continuously adjustable from an infrared band to an ultraviolet band, and meanwhile, the InGaN material has the advantages of direct band gap, high electron mobility, good mechanical and chemical stability, excellent radiation resistance, excellent temperature characteristic and the like, so that the InGaN material is widely concerned in the field of photoelectrons. In recent years, InGaN materials have enjoyed great success in the fields of solid state lighting, ultraviolet sterilization, visible light communication, LED display, and the like. However, In the InGaN-based optoelectronic device, the crystal quality of the InGaN material is rapidly reduced with the gradual increase of the In component, and the application of the high In component InGaN material is greatly limited.
The preparation of high-quality and high-In-content InGaN material is still very difficult, mainly because: the InGaN material is mainly prepared on a GaN substrate or a template by an epitaxial method at present, lattice mismatch between an epitaxial layer and the substrate can generate a large amount of mismatch dislocation, and huge pressure stress can be introduced in the epitaxial process of an InGaN film and a quantum structure; secondly, with the increase of the In component, the growth temperature of the InGaN material is gradually reduced, so that the ammonia gas cracking efficiency is insufficient, and the migration distance of atoms on the surface of the substrate is insufficient, so that the quality of the epitaxial crystal of the high-In component InGaN material is poor.
The key to improving the epitaxial crystal quality of InGaN thin films and quantum structures In InGaN-based optoelectronic devices is to improve the incorporation efficiency of In atoms and then improve the epitaxial growth temperature of InGaN materials. Theoretical calculations indicate that the incorporation efficiency of In atoms is highest when the GaN substrate or template is In a state of weak tensile stress. Various schemes have been proposed internationally for releasing compressive stress In GaN heteroepitaxial films, such as two-dimensional material transition layers, porous GaN templates, InGaNOS templates, etc., and experimental results also demonstrate that by releasing compressive stress present In GaN films, the crystal quality of high In component InGaN materials is significantly improved. However, these methods are complicated in process, expensive in cost, and not fully compatible with the existing preparation method of InGaN materials, and thus they still remain in the laboratory development stage, and still have a distance from practical application.
Disclosure of Invention
In view of the above, it is necessary to provide an InGaN-based optoelectronic device and a method for manufacturing the same, aiming at the technical problem of how to improve the incorporation efficiency of In component In the InGaN-based optoelectronic device.
A preparation method of an InGaN-based optoelectronic device comprises the following steps:
forming an AlN transition layer on the crystal substrate by adopting a physical vapor deposition method, wherein the AlN transition layer consists of a plurality of first three-dimensional growth islands;
epitaxially growing a GaN transition layer on the AlN transition layer, wherein the GaN transition layer consists of a plurality of second three-dimensional growth small islands, and the plurality of second three-dimensional growth small islands in the GaN transition layer are the continuations of the plurality of first three-dimensional growth small islands in the AlN transition layer, so as to obtain a composite substrate of the InGaN-based optoelectronic device;
epitaxially growing a nitride conversion layer on the composite substrate of the InGaN-based optoelectronic device in a two-dimensional epitaxial mode, so that grain boundaries of the second three-dimensional growth island in the GaN transition layer are merged, and providing tensile stress formed by grain boundary merging induction in the nitride conversion layer; and
and forming other device structure layers of the InGaN-based optoelectronic device on the nitride conversion layer to obtain the InGaN-based optoelectronic device.
The preparation method of the InGaN-based optoelectronic device is simple In process, the AlN transition layer and the GaN transition layer form the composite transition layer In the preparation process, the stress state In the nitride conversion layer can be modulated, the incorporation efficiency of In atoms In the InGaN material In the InGaN-based optoelectronic device In the epitaxial process is improved, and therefore the quality of an InGaN film and epitaxial crystals of quantum structures is improved. The preparation method of the InGaN-based optoelectronic device has high compatibility with the epitaxial process of the existing commercial InGaN-based optoelectronic device, and the preparation method of the InGaN-based optoelectronic device is easy to be directly applied to large-scale industrial production.
In one possible implementation, the operation of forming the AlN transition layer on the crystal substrate by physical vapor deposition is: sputtering a target material with the purity of more than or equal to 99.99 percent on a crystal substrate to form an AlN transition layer in the mixed atmosphere of argon and nitrogen; wherein the working pressure is 0.1 Pa-1 Pa, the volume fraction of nitrogen in the mixed atmosphere is 10% -90%, the temperature of the crystal substrate is 20-800 ℃, and the sputtering power is 1000-5000W.
In a feasible realization mode, in the operation of epitaxially growing the GaN transition layer on the AlN transition layer, the growth temperature is 500-600 ℃.
In one possible implementation, the growth temperature in the operation of epitaxially growing a nitride conversion layer in a two-dimensional epitaxial mode on the composite substrate of the InGaN-based optoelectronic device is 600 to 1200 ℃.
In one possible implementation, the AlN transition layer has a thickness of 0.5nm to 500 nm.
In one possible implementation, the thickness of the GaN transition layer is 0.5nm to 500 nm.
In one possible implementation, the crystal substrate is selected from at least one of a sapphire substrate, a gallium nitride substrate, an aluminum nitride substrate, a silicon carbide substrate, and a gallium oxide substrate.
In one possible implementation, the nitride conversion layer is a GaN layer, an AlN layer, an AlGaN layer, or an InGaN layer; and/or the thickness of the nitride conversion layer is 0.1-10 μm.
An InGaN-based optoelectronic device is prepared by any one of the preparation methods of the InGaN-based optoelectronic device.
The In atom incorporation efficiency In the InGaN material epitaxy process In the InGaN-based optoelectronic device is high, so that the quality of an InGaN film and an epitaxial crystal with a quantum structure is improved, and the overall efficiency of the InGaN-based optoelectronic device is high.
In one possible implementation, the InGaN-based optoelectronic device is an InGaN-based LED, an InGaN-based solar cell, or an InGaN-based laser.
Drawings
Fig. 1 is a flow chart of a method of fabricating an InGaN-based optoelectronic device in accordance with an embodiment of the present invention;
fig. 2 is a schematic view of a composite substrate of an InGaN-based optoelectronic device in accordance with an embodiment of the present invention;
fig. 3 is a schematic view of a template for an InGaN-based optoelectronic device in accordance with an embodiment of the present invention;
fig. 4 is a schematic diagram of an InGaN-based optoelectronic device in accordance with an embodiment of the present invention;
fig. 5 is a schematic view of an InGaN-based optoelectronic device of comparative example 1;
fig. 6 is a schematic view of an InGaN-based optoelectronic device of comparative example 2;
fig. 7 is an atomic force microscope image of the GaN transition layer surface of the InGaN-based optoelectronic device of example 1;
fig. 8 is an atomic force microscope image of the AlN transition layer surface of the InGaN-based optoelectronic device of comparative example 1;
fig. 9 is an atomic force microscope image of the surface of the GaN transition layer of the InGaN-based optoelectronic device of comparative example 2;
FIG. 10 is the reflectance recorded during epitaxial growth in steps 5) to 6) of example 1 and steps 4) to 5) of comparative example 1 and comparative example 2;
FIG. 11 is an in-situ warpage monitoring curve recorded during epitaxial growth in steps 5) to 6) of example 1 and steps 4) to 5) of comparative example 1 and comparative example 2;
fig. 12 is an electroluminescence spectrum of InGaN-based optoelectronic devices of example 1 and comparative example 1.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, a method for manufacturing an InGaN-based optoelectronic device according to an embodiment of the present invention includes the following steps:
and S1, forming an AlN transition layer on the crystal substrate by adopting a physical vapor deposition method, wherein the AlN transition layer consists of a plurality of first three-dimensional growth islands.
Referring to fig. 2, in step S1, the crystal substrate 110 refers to a substrate made of crystal, and the crystal substrate 110 is used to support other layers on the upper layer.
In one possible implementation, the crystal substrate 110 is selected from at least one of a sapphire substrate, a gallium nitride substrate, an aluminum nitride substrate, a silicon carbide substrate, and a gallium oxide substrate. That is, the crystal substrate 110 may be a single-layer sapphire substrate, a gallium nitride substrate, an aluminum nitride substrate, a silicon carbide substrate, or a gallium oxide substrate, or may be a multi-layer substrate formed by stacking a plurality of substrates made of the same material or different materials.
In step S1, AlN transition layer 120 formed on crystal substrate 110 using a physical vapor deposition method is composed of a large number of dense crystal grains (i.e., first three-dimensionally grown islands), and the c-axis orientations of the crystal grains have a high degree of uniformity. AlN transition layer 120 provides an initial growth state that increases the uniformity of grain orientation in a certain direction. In addition, the AlN transition layer 120 can also prevent Ga from corroding the crystal base 110 when GaN is subsequently grown. The technological parameters of the film deposition and the deposition time can be adjusted to realize the regulation and control of the thickness, the surface appearance and the crystal quality of the AlN transition layer. The AlN transition layer can also be annealed at high temperature to improve the crystallization quality.
In one possible implementation, the operation of forming AlN transition layer 120 on crystal substrate 110 by physical vapor deposition is: sputtering a target material with the purity of more than or equal to 99.99 percent on a crystal substrate to form an AlN transition layer in the mixed atmosphere of argon and nitrogen; wherein the working pressure is 0.1 Pa-1 Pa, the volume fraction of nitrogen in the mixed atmosphere is 10% -90%, the temperature of the crystal substrate is 20-800 ℃, and the sputtering power is 1000-5000W. Wherein, the material of the target material can be high-purity aluminum; the argon in the mixed atmosphere is a sputtering gas, which can be high-purity argon, and the nitrogen is a reaction gas, which can be high-purity nitrogen. Specifically, high-purity argon is used as sputtering gas to discharge to form ions, and the ions bombard high-purity aluminum used as a sputtering target after being accelerated by an electric field, so that aluminum atoms of the target are sputtered out to form aluminum nitride with high-purity nitrogen used as reaction gas to be deposited on the surface of a heated crystal substrate.
In one possible implementation, AlN transition layer 120 has a thickness in the range of 0.5nm to 500 nm. For example, the AlN transition layer 120 may have a thickness of 0.5nm, 1nm, 5nm, 10nm, 50nm, 100nm, 200nm, 300nm, 400nm, or 500 nm.
And S2, epitaxially growing a GaN transition layer on the AlN transition layer, wherein the GaN transition layer consists of a plurality of second three-dimensional growth small islands, and the plurality of second three-dimensional growth small islands in the GaN transition layer are the continuations of the plurality of first three-dimensional growth small islands in the AlN transition layer, so that the composite substrate of the InGaN-based optoelectronic device is obtained.
Referring to fig. 2, in step S2, the heteroepitaxial substrate coated with the AlN transition layer 120 may be loaded on a heating susceptor of an epitaxial apparatus, the GaN transition layer 130 may be epitaxially prepared on the AlN transition layer 120 at a suitable temperature and under other process parameters, and the size and grain boundary density of the second three-dimensional growth island in the GaN transition layer 130 may be controlled by controlling the process conditions and growth time of the GaN transition layer 130.
The epitaxial apparatus may be Metal Organic Chemical Vapor Deposition (MOCVD), Molecular Beam Epitaxy (MBE), Hydride Vapor Phase Epitaxy (HVPE), or other types of epitaxial apparatuses. The process conditions include temperature, chamber pressure, V/III ratio, substrate pedestal rotation speed, source flow, etc.
In one possible implementation, the GaN transition layer 130 is epitaxially grown on the AlN transition layer 120 at a growth temperature of 500 to 600 ℃. At this time, the formation of the second three-dimensionally grown islands and grain boundaries in the GaN buffer layer 130 can be promoted.
In one possible implementation, the thickness of the GaN buffer layer 130 is 0.5nm to 500 nm. For example, the thickness of the GaN transition layer 130 may be 0.5nm, 1nm, 5nm, 10nm, 50nm, 100nm, 200nm, 300nm, 400nm, or 500 nm.
Through step S2, the composite substrate 100 of an InGaN-based optoelectronic device shown in fig. 2 can be obtained.
And S3, epitaxially growing a nitride conversion layer in a two-dimensional epitaxial mode on the composite substrate of the InGaN-based optoelectronic device, merging the grain boundaries of the second three-dimensional growth island in the GaN transition layer, and providing tensile stress induced by merging of the grain boundaries in the nitride conversion layer.
Referring to fig. 3 together, in step S3, in the process of epitaxially growing the nitride conversion layer 210 in the two-dimensional epitaxial mode on the composite substrate 100 of the InGaN-based optoelectronic device, the AlN transition layer 120 can be rapidly merged by the grain boundaries of the first three-dimensional growth islands and the second three-dimensional growth island in the GaN transition layer 130. Meanwhile, the tensile stress formed by grain boundary combination induction is provided in the continuous epitaxial film (namely the nitride conversion layer), so that the stress state in the nitride hetero-epitaxial film is modulated.
In one possible implementation, the growth temperature during the operation of epitaxially growing the nitride conversion layer 210 is 600 ℃ to 1200 ℃. In this step, the stress state in the continuous nitride conversion layer 210 can be monitored in real time by monitoring the warpage of the composite substrate 100 of the InGaN-based optoelectronic device in situ.
In one possible implementation, the thickness of the nitride conversion layer 210 is 0.1 μm to 10 μm.
Through step S3, the template 200 of the InGaN-based optoelectronic device shown in fig. 3 can be obtained. The template 200 of the InGaN-based optoelectronic device includes a composite substrate 100 and a nitride conversion layer 210 of the InGaN-based optoelectronic device in order from bottom to top. The composite substrate 100 of the InGaN-based optoelectronic device sequentially includes a crystal base 110, an AlN transition layer 120, and a GaN transition layer 130 from bottom to top.
And S4, forming other device structure layers of the InGaN-based optoelectronic device on the nitride conversion layer to obtain the InGaN-based optoelectronic device.
In step S4, other device structure layers may be formed on the nitride conversion layer by processes commonly used in the art, and may be selected according to the specific InGaN-based optoelectronic device.
Referring to fig. 4 together, in one possible implementation, the InGaN-based optoelectronic device 300 is an InGaN-based red LED, and other device structure layers of the InGaN-based optoelectronic device include an n-type GaN layer 310, an InGaN/GaN multi-quantum well layer 320, and a p-type GaN layer 330.
The preparation method of the InGaN-based optoelectronic device is simple In process, the AlN transition layer and the GaN transition layer form the composite transition layer In the preparation process, the stress state In the nitride conversion layer can be modulated, and the incorporation efficiency of In atoms In the InGaN material epitaxy process In the InGaN-based optoelectronic device is improved, so that the quality of the InGaN film and the epitaxial crystal of the quantum structure is improved. The preparation method of the InGaN-based optoelectronic device has high compatibility with the epitaxial process of the existing commercial InGaN-based optoelectronic device, and the preparation method of the InGaN-based optoelectronic device is easy to be directly applied to large-scale industrial production.
Referring to fig. 4, an InGaN-based optoelectronic device 300 according to an embodiment of the present invention is prepared by any of the above methods for preparing an InGaN-based optoelectronic device.
In one possible implementation manner, the InGaN-based optoelectronic device 300 is an InGaN-based red LED, and sequentially includes, from bottom to top, a template 200 of the InGaN-based optoelectronic device, an n-type GaN layer 310, an InGaN/GaN multi-quantum well layer 320, and a p-type GaN layer 330. The template 200 of the InGaN-based optoelectronic device sequentially comprises a composite substrate 100 of the InGaN-based optoelectronic device and a nitride conversion layer 210 from bottom to top. The composite substrate 100 of the InGaN-based optoelectronic device sequentially includes a crystal base 110, an AlN transition layer 120, and a GaN transition layer 130 from bottom to top.
Of course, the InGaN-based optoelectronic device of the present invention is not limited to the InGaN-based LED described above, but may also be an InGaN-based solar cell or an InGaN-based laser.
Further, the InGaN-based optoelectronic device 300 of the present invention includes a high In composition InGaN thin film and quantum structure and associated ancillary structures, wherein the high In composition InGaN thin film and quantum structure and associated ancillary structures may be a current injection layer and an active region structure of an optoelectronic device such as a long wavelength InGaN-based LED, an InGaN-based solar cell, a long wavelength InGaN-based laser, or other forms of ancillary structures.
The In atom incorporation efficiency In the InGaN material epitaxy process In the InGaN-based optoelectronic device is high, so that the quality of an InGaN film and an epitaxial crystal with a quantum structure is improved, and the overall efficiency of the InGaN-based optoelectronic device is high.
In order to make the technical solution of the present application more specific, clear and easy to understand by referring to the above implementation, the technical solution of the present application is exemplified, but it should be noted that what the present application is to protect is not limited to the following embodiment 1.
Example 1
Referring to fig. 4, the InGaN-based optoelectronic device 300 of embodiment 1 is an InGaN-based red light emitting diode, and sequentially includes, from bottom to top, a template 200 of the InGaN-based optoelectronic device, an n-type GaN layer 310, an InGaN/GaN multi-quantum well layer 320, and a p-type GaN layer 330. The template 200 of the InGaN-based optoelectronic device sequentially comprises a composite substrate 100 of the InGaN-based optoelectronic device and a nitride conversion layer 210 from bottom to top, wherein the nitride conversion layer 210 is made of GaN. The composite substrate 100 of the InGaN-based optoelectronic device sequentially comprises a crystal base 110, an AlN transition layer 120 and a GaN transition layer 130 from bottom to top, wherein the crystal base 110 is made of c-plane sapphire.
The preparation method of the InGaN-based red light emitting diode of embodiment 1 includes the following steps:
1) high-purity argon is used as sputtering gas to discharge to form ions, high-purity aluminum (the purity is more than or equal to 99.99%) used as a sputtering target is bombarded after being accelerated by an electric field, aluminum atoms of the target are sputtered out to form aluminum nitride with high-purity nitrogen used as reaction gas, the aluminum nitride is deposited on a heated crystal substrate 110, an AlN transition layer 120 with the thickness of 25nm is obtained, the working pressure in the process is 0.67Pa, the volume fraction of the nitrogen is 25%, the temperature of the crystal substrate 110 is 550 ℃, and the sputtering power is 3000W. The AlN transition layer 120 is formed to consist of a large number of dense first three-dimensionally grown islands, and the first three-dimensionally grown islands have a high degree of uniformity in c-axis orientation.
2) And ultrasonically cleaning the crystal substrate 110 plated with the AlN transition layer 120 in acetone, alcohol and deionized water for 10min respectively, and then blow-drying the surface by using dry nitrogen.
3) And loading the dried crystal substrate 110 plated with the AlN transition layer 120 on a heating base of MOCVD equipment, heating to 1080 ℃, and then performing a high-temperature surface thermal cleaning process in a hydrogen atmosphere for 10 min.
4) And cooling the heating base to 550 ℃, introducing trimethyl gallium and ammonia gas into the reaction chamber, and preparing a GaN transition layer 130 consisting of second three-dimensional growth islands on the AlN transition layer 120 to obtain the composite substrate 100 of the InGaN-based optoelectronic device. In the present embodiment, the thickness of the GaN buffer layer 130 is 5 nm.
5) And raising the temperature of the heating base to 1075 ℃, setting the pressure of the MOCVD cavity to 200torr, the V/III ratio to 2500 and the rotating speed of the heating base to 1200rpm, epitaxially preparing a continuous nitride conversion layer 210 on the GaN/AlN composite transition layer in a two-dimensional epitaxial mode, enabling the grain boundaries in the GaN transition layer 130 to be rapidly combined, and providing tensile stress formed by combining and inducing the grain boundaries in the nitride conversion layer 210 to obtain the template 200 of the InGaN-based optoelectronic device. In the present embodiment, the thickness of the nitride conversion layer 210 is 2 μm.
6) On the basis of the step 5), setting the temperature of the heating base to 1060 ℃, the pressure of the MOCVD cavity to be 200torr, the V/III ratio to be 2500 and the rotating speed of the heating base to be 1200rpm, and epitaxially growing an n-type GaN layer 310 to be used as a first conductive type current injection layer of the InGaN-based red light emitting diode. In the present embodiment, the thickness of the n-type GaN layer 310 is 2 μm.
7) On the basis of the step 6), setting the pressure of an MOCVD cavity to be 200torr, the V/III ratio to be 4000 and the rotating speed of a heating base to be 1200rpm, and epitaxially growing an InGaN/GaN multi-quantum well layer 320 in a nitrogen carrier gas atmosphere to serve as a light emitting active region of the InGaN red light LED, wherein the growth temperature of the InGaN well layer is 700 ℃ and the growth temperature of the GaN barrier layer is 800 ℃; setting the temperature of the heating base to 950 ℃, the pressure of the MOCVD cavity to 200torr, the V/III ratio to 2500 and the rotation speed of the heating base to 1200rpm, epitaxially preparing a p-type GaN layer 330 as a current injection layer of the second conductivity type of the InGaN-based red light emitting diode, and obtaining the InGaN-based optoelectronic device 300 of the embodiment 1.
Comparative example 1
Referring to fig. 5, the InGaN-based optoelectronic device 100 'of comparative example 1 is an InGaN-based red light emitting diode, and sequentially includes, from bottom to top, a sapphire substrate 110', an AlN transition layer 120 ', a GaN conversion layer 130', an n-type GaN layer 140 ', an InGaN/GaN multiple quantum well layer 150', and a p-type GaN layer 160 ', wherein the sapphire substrate 110' is made of c-plane sapphire.
The preparation method of the InGaN-based red light emitting diode of comparative example 1 includes the steps of:
1) high-purity argon is used as sputtering gas to discharge to form ions, high-purity aluminum (the purity is more than or equal to 99.99%) used as a sputtering target is bombarded after being accelerated by an electric field, so that target aluminum atoms are sputtered out to form aluminum nitride with the high-purity nitrogen used as reaction gas, the aluminum nitride is deposited on a heated sapphire substrate 110 ', an AlN transition layer 120 ' with the thickness of 25nm is obtained, the working pressure in the process is 0.67Pa, the volume fraction of the nitrogen is 25%, the temperature of the sapphire substrate 110 ' is 550 ℃, and the sputtering power is 3000W. The AlN transition layer 120' formed is composed of a large number of dense first three-dimensionally grown islands, and the first three-dimensionally grown islands have a high degree of uniformity in c-axis orientation.
2) And ultrasonically cleaning the sapphire substrate 110 'plated with the AlN transition layer 120' in acetone, alcohol and deionized water for 10min respectively, and then drying the surface by dry nitrogen.
3) And loading the dried AlN transition layer 120 'plated sapphire substrate 110' onto a heating base of MOCVD equipment, heating to 1080 ℃, and then performing a high-temperature surface thermal cleaning process in a hydrogen atmosphere for 10 min.
4) The temperature of the heated susceptor was adjusted to 1075 ℃, the MOCVD chamber pressure was set to 200torr, the V/III ratio was 2500, and the heated susceptor rotation speed was 1200rpm, and a continuous GaN conversion layer 130' was epitaxially prepared on the AlN transition layer in a two-dimensional epitaxial mode. In this comparative example, the thickness of GaN conversion layer 130' was 2 μm.
5) On the basis of the step 4), setting the temperature of the heating base to 1060 ℃, the pressure of the MOCVD cavity to 200torr, the V/III ratio to 2500 and the rotating speed of the heating base to 1200rpm, and using the n-type GaN layer 140' as a first conduction type current injection layer of the InGaN-based red light emitting diode. In this comparative example, the thickness of the n-type GaN layer was 2 μm.
6) Setting the pressure of an MOCVD cavity to be 200torr, the V/III ratio to be 4000 and the rotating speed of a heating base to be 1200rpm on the basis of the step 5), and epitaxially growing an InGaN/GaN multi-quantum well layer 150' in a nitrogen carrier gas atmosphere to serve as a light emitting active region of the InGaN red light LED, wherein the growth temperature of the InGaN well layer is 700 ℃ and the growth temperature of the GaN barrier layer is 800 ℃; setting the temperature of the heating base to 950 ℃, the pressure of the MOCVD cavity to 200torr, the V/III ratio to 2500 and the rotating speed of the heating base to 1200rpm, and epitaxially preparing a p-type GaN layer 160 'to be used as a current injection layer of a second conductive type of the InGaN-based red light emitting diode to obtain the InGaN-based optoelectronic device 100' of the comparative example 1.
Comparative example 2
Referring to fig. 6, the InGaN-based optoelectronic device 200 'of comparative example 2 is an InGaN-based red light emitting diode, and sequentially includes, from bottom to top, a sapphire substrate 210', a GaN transition layer 220 ', a GaN conversion layer 230', an n-type GaN layer 240 ', an InGaN/GaN multiple quantum well layer 250', and a p-type GaN layer 260 ', wherein the sapphire substrate 210' is made of c-plane sapphire.
The preparation method of the InGaN-based red light emitting diode of comparative example 2 includes the steps of:
1) sapphire substrate 210' was ultrasonically cleaned in acetone, alcohol, and deionized water for 10min each, and the substrate surface was blow-dried with dry nitrogen.
2) And loading the dried sapphire substrate 210' on a heating base of MOCVD equipment, heating to 1080 ℃, and then carrying out a high-temperature surface thermal cleaning process for 10min in a hydrogen atmosphere.
3) The heating base is cooled to 550 ℃, trimethyl gallium and ammonia gas are introduced into the reaction chamber, and as shown in fig. 2, a GaN transition layer 220 'composed of three-dimensional growth islands is prepared on the sapphire substrate 210'. In this comparative example, the thickness of the GaN transition layer 220' was 5 nm.
4) The temperature of the heated susceptor was raised to 1075 ℃, the MOCVD chamber pressure was set to 200torr, the V/III ratio was 2500, and the heated susceptor rotation speed was 1200rpm, and a continuous GaN conversion layer 230 'was epitaxially prepared in a two-dimensional epitaxial mode on the GaN transition layer 220'. In this comparative example, the thickness of the GaN conversion layer 230' was 2 μm.
5) On the basis of the step 4), setting the temperature of the heating base to 1060 ℃, the pressure of the MOCVD cavity to be 200torr, the V/III ratio to be 2500 and the rotating speed of the heating base to be 1200rpm, and epitaxially growing an n-type GaN layer 240' to be used as a first conductive type current injection layer of the InGaN-based red light emitting diode. In the present comparative example, the thickness of the n-type GaN layer 240' was 2 μm.
6) Setting the pressure of an MOCVD cavity to be 200torr, the V/III ratio to be 4000 and the rotating speed of a heating base to be 1200rpm on the basis of the step 5), and epitaxially growing an InGaN/GaN multi-quantum well layer 250' in a nitrogen carrier gas atmosphere to serve as a light emitting active region of the InGaN red light LED, wherein the growth temperature of the InGaN well layer is 700 ℃ and the growth temperature of the GaN barrier layer is 800 ℃; setting the temperature of the heating base to 950 ℃, the pressure of the MOCVD cavity to 200torr, the V/III ratio to 2500 and the rotation speed of the heating base to 1200rpm, epitaxially preparing a p-type GaN layer 260 'as a current injection layer of a second conductivity type of the InGaN-based red light emitting diode, and obtaining the InGaN-based optoelectronic device 200' of the comparative example 2.
And (3) performance testing:
the surface of the GaN transition layer of the InGaN-based optoelectronic device of example 1, the surface of the AlN transition layer of the InGaN-based optoelectronic device of comparative example 1, and the surface of the GaN transition layer of the InGaN-based optoelectronic device of comparative example 2 were respectively subjected to atomic force microscope scanning, to obtain fig. 7 to 9. As can be seen from fig. 7 to 9, the transition layers of different structures have different surface morphology characteristics, the GaN transition layer of the InGaN-based optoelectronic device of example 1 is composed of second three-dimensional growth islands with larger size, the three-dimensional islands are connected with each other and have voids, the AlN transition layer of the InGaN-based optoelectronic device of comparative example 1 is a dense quasi-continuous thin film composed of three-dimensional growth islands with smaller size, and the GaN transition layer of the InGaN-based optoelectronic device of comparative example 2 is composed of three-dimensional growth islands with smaller size and lower density.
The reflectivity and warpage during epitaxial growth of steps 5) to 6) in example 1 and steps 4) to 5) in comparative example 1 and 2) were monitored in situ, yielding fig. 10 and 11. As can be seen from FIGS. 10 and 11, in the case of using the GaN transition layer in comparative example 2, the continuous GaN thin film described in steps 4 to 5) of comparative example 2 could not be prepared in the two-dimensional epitaxial mode. From the warpage in-situ monitoring curves of example 1 and comparative example 1, it can be deduced that the magnitudes of tensile stresses in the n-type GaN layer of example 1 and the n-type GaN layer of comparative example 1 are 1.72GPa and 1.51GPa, respectively.
The electroluminescence spectra of the InGaN-based optoelectronic devices of example 1 and comparative example 1 are shown in fig. 12. As can be seen from fig. 12, the LED epitaxial structure for preparing an InGaN-based optoelectronic device In example 1 using the GaN/AlN composite transition layer has a longer emission wavelength, i.e., higher In component incorporation efficiency.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, many variations and modifications can be made without departing from the spirit of the invention, which falls within the scope of the invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (10)
1. A preparation method of an InGaN-based optoelectronic device is characterized by comprising the following steps:
forming an AlN transition layer on the crystal substrate by adopting a physical vapor deposition method, wherein the AlN transition layer consists of a plurality of first three-dimensional growth islands;
epitaxially growing a GaN transition layer on the AlN transition layer, wherein the GaN transition layer consists of a plurality of second three-dimensional growth small islands, and the plurality of second three-dimensional growth small islands in the GaN transition layer are the continuations of the plurality of first three-dimensional growth small islands in the AlN transition layer, so as to obtain a composite substrate of the InGaN-based optoelectronic device;
epitaxially growing a nitride conversion layer on the composite substrate of the InGaN-based optoelectronic device in a two-dimensional epitaxial mode, so that grain boundaries of the second three-dimensional growth island in the GaN transition layer are merged, and providing tensile stress formed by grain boundary merging induction in the nitride conversion layer; and
and forming other device structure layers of the InGaN-based optoelectronic device on the nitride conversion layer to obtain the InGaN-based optoelectronic device.
2. The method of fabricating an InGaN-based optoelectronic device as set forth in claim 1, wherein the forming of the AlN transition layer on the crystal substrate by physical vapor deposition is performed by: sputtering a target material with the purity of more than or equal to 99.99 percent on a crystal substrate to form an AlN transition layer in the mixed atmosphere of argon and nitrogen; wherein the working pressure is 0.1 Pa-1 Pa, the volume fraction of nitrogen in the mixed atmosphere is 10% -90%, the temperature of the crystal substrate is 20-800 ℃, and the sputtering power is 1000-5000W.
3. The method for manufacturing an InGaN-based optoelectronic device according to claim 1, wherein the growth temperature in the operation of epitaxially growing the GaN transition layer on the AlN transition layer is 500 to 600 ℃.
4. The method of manufacturing an InGaN-based optoelectronic device according to claim 1, wherein the growth temperature in the operation of epitaxially growing the nitride epitaxial layer in the two-dimensional epitaxial mode on the composite substrate of the InGaN-based optoelectronic device is 600 to 1200 ℃.
5. The method of fabricating an InGaN-based optoelectronic device of claim 1, wherein the AlN transition layer has a thickness of 0.5nm to 500 nm.
6. The method of claim 1, wherein the GaN transition layer has a thickness of 0.5nm to 500 nm.
7. The method of manufacturing an InGaN-based optoelectronic device of claim 1, wherein the crystal substrate is at least one selected from a sapphire substrate, a gallium nitride substrate, an aluminum nitride substrate, a silicon carbide substrate, and a gallium oxide substrate.
8. The method of manufacturing an InGaN-based optoelectronic device according to claim 1, wherein the nitride epitaxial layer is a GaN layer, an AlN layer, an AlGaN layer, or an InGaN layer; and/or the thickness of the nitride epitaxial layer is 0.1-10 μm.
9. An InGaN-based optoelectronic device, characterized in that the InGaN-based optoelectronic device is prepared by the method of any one of claims 1 to 8.
10. InGaN-based optoelectronic device according to claim 9, wherein the InGaN-based optoelectronic device is an InGaN-based LED, an InGaN-based solar cell or an InGaN-based laser.
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