CN114242855A - Light emitting diode epitaxial wafer and preparation method thereof - Google Patents
Light emitting diode epitaxial wafer 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
- H01L33/0066—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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- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
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- 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
- C30B25/06—Epitaxial-layer growth by reactive sputtering
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- 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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- 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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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- 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
- H01L33/325—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen characterised by the doping materials
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Abstract
The invention discloses a light-emitting diode epitaxial wafer and a preparation method thereof.A first AlGaN layer is subjected to plasma treatment, and plasma can react with an N vacancy defect state surface layer on the surface of the first AlGaN layer to form a plasma treatment layer with high crystal quality and stable structure, so that the problem of poor quality of the N vacancy defect state surface layer on the original first AlGaN layer is solved, the crystal quality of the epitaxial layer is further improved, and the luminous efficiency is further improved; meanwhile, in the plasma treatment process, oxygen atoms diffused on the substrate can be adsorbed by the active plasma, so that the content of the oxygen atoms on the first AlGaN layer is reduced, the oxygen atoms are prevented from extending and diffusing into the multiple quantum well layer, and the luminous efficiency is further improved.
Description
Technical Field
The invention relates to the technical field of semiconductor devices, in particular to a light-emitting diode epitaxial wafer and a preparation method thereof.
Background
In recent years, AlGaN materials are receiving attention due to their great application potential in ultraviolet photoelectric devices, and ultraviolet LEDs have the characteristics of high photon energy, short wavelength, small size, low power consumption, long service life, environmental friendliness, and the like, and have wide applications in the fields of high color rendering index white light illumination, high-density optical data storage, sensors, lithography, air purification, environmental protection, and the like.
Currently, when an AlGaN layer is prepared in an epitaxial wafer structure, NH is generally adopted3The reaction was carried out under ambient conditions, but with increasing Al content, Al and NH3The pre-reaction is more severe, so that the epitaxial growth AlGaN layer has more N vacancy defects, the problems of high defect density and uneven surface of the AlGaN layer film are caused, the crystal quality of the AlGaN layer is not as good as that of the GaN layer, and the luminous efficiency of the ultraviolet LED is not high; meanwhile, oxygen atoms decomposed from the oxide on the surface of the substrate at high temperature can be upwards diffused along with the growth of the epitaxial layer, and when the oxygen atoms are diffused to the quantum well layer, carriers can be absorbed to a certain extent, so that the radiation recombination efficiency of the carriers in the quantum well layer is reduced, and the light emitting efficiency of the ultraviolet LED is further low.
Therefore, how to improve the luminous efficiency of the ultraviolet LED becomes a problem that improvement is needed in the existing ultraviolet LED technology.
Disclosure of Invention
The application aims to provide a light-emitting diode epitaxial wafer and a preparation method thereof, so as to solve the problem of how to improve the luminous efficiency of an ultraviolet LED.
The scheme adopted by the application to solve the technical problems is as follows:
in a first aspect, the application provides a light emitting diode epitaxial wafer, be in including substrate and setting lamination on the substrate, lamination includes first AlGaN layer and the multiple quantum well layer that sets up from bottom to top at least, first AlGaN layer is close to one side of multiple quantum well layer is provided with plasma treatment layer, plasma treatment layer is made for the top layer and the plasma reaction on first AlGaN layer, the top layer is N vacancy defect state top layer.
In some embodiments of the present application, the plasma is a nitrogen-containing plasma and the plasma treated layer is a GaN thin film.
In some embodiments of the present application, the first AlGaN layer includes an undoped AlGaN layer and an N-type doped AlGaN layer from bottom to top in sequence, and the plasma treatment layer is grown on a side of the N-type doped AlGaN layer away from the undoped AlGaN layer.
In some embodiments of the present application, the N-doped AlGaN layer comprises an N-vacancy defect state skin layer, and the plasma treatment layer is formed by reacting the plasma with the N-vacancy defect state skin layer.
In some embodiments of the present application, the plasma is N2And (4) O plasma.
In a second aspect, the present application further provides a method for preparing an epitaxial wafer of a light emitting diode, including the following steps:
providing a substrate;
preparing a laminated structure on a substrate, wherein the laminated structure at least comprises a first AlGaN layer and a multi-quantum well layer which are arranged from bottom to top;
after the first AlGaN layer is prepared, carrying out plasma treatment on one side, close to the multi-quantum well layer, of the first AlGaN layer to form a plasma treatment layer;
the plasma processing step comprises the step of reacting plasma with the N-vacancy defect state surface layer of the first AlGaN layer to generate a plasma processing layer.
In some embodiments of the present application, in the step of preparing the first AlGaN layer, the method further includes the steps of:
growing an undoped AlGaN layer on the buffer layer at a high temperature;
and growing an N-type doped AlGaN layer on the undoped AlGaN layer, wherein the N-type doped AlGaN layer is doped with Si.
In some embodiments of the present application, in the step of preparing the plasma treatment layer, the substrate of the grown N-type doped AlGaN layer is placed at a negative electrode position in a magnetron sputtering system, and a plasma containing nitrogen plasma is introduced at a positive electrode position of the system, so that the plasma reacts with the N-vacancy defect state surface layer of the N-type doped AlGaN layer to form a GaN film.
In some embodiments of the present application, the method comprises the following steps:
providing a sapphire Al2O3A substrate; growing a buffer layer on the substrate by adopting a physical vapor deposition method, and carrying out in-situ annealing treatment on the buffer layer; after the annealing is finished, growing an undoped AlGaN layer on the buffer layer at a high temperature, wherein the Al component is between 30 and 80 percent; growing a Si-doped N-type doped AlGaN layer on the undoped AlGaN layer, wherein the Al component is between 20 and 60 percent; introducing N on the N-type doped AlGaN layer2O plasma, preparing a plasma treatment layer by adopting a radio frequency controlled sputtering method; preparing a multi-quantum well layer on the plasma processing layer by an MOCVD method, wherein the multi-quantum well layer is GaN/AlGaN with 5 to 12 periods, GaN is a well layer, and AlGaN is a barrier layer; growing an AlGaN electronic barrier layer on the multi-quantum well layer; and growing a P-type doped GaN layer on the electron blocking layer, wherein the doping element is Mg.
In some embodiments of the present application, growing an AlGaN contact layer on the P-type doped GaN layer, and annealing the entire epitaxial structure after the contact layer is prepared.
According to the light-emitting diode epitaxial wafer and the preparation method thereof, the first AlGaN layer is subjected to plasma treatment, and the plasma can react with the N vacancy defect state surface layer on the surface of the first AlGaN layer to form a plasma treatment layer with high crystal quality and stable structure, so that the problem that the quality of the N vacancy defect state surface layer on the original first AlGaN layer is poor is solved, the crystal quality of the epitaxial layer is further improved, and the luminous efficiency is further improved; meanwhile, in the plasma treatment process, oxygen atoms diffused on the substrate can be adsorbed by the active plasma, so that the content of the oxygen atoms on the first AlGaN layer is reduced, the oxygen atoms are prevented from extending and diffusing into the multiple quantum well layer, and the luminous efficiency is further improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a view showing the structure of an epitaxial wafer according to the present invention;
fig. 2 is a process diagram of the epitaxial wafer fabrication method of the present invention.
Description of the element symbols:
the solar cell comprises a substrate 1, a buffer layer 2, an undoped AlGaN layer 3, an N-type doped AlGaN layer 4, a plasma treatment layer 5, a multi-quantum well layer 6, an electron blocking layer 7, a P-type doped GaN layer 8 and a contact layer 9.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly and completely with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only some embodiments, not all embodiments, of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and for simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be considered as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or including indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the described features. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present application, the word "exemplary" is used to mean "serving as an example, instance, or illustration. Any embodiment described herein as exemplary is not necessarily to be construed as preferred or advantageous over other embodiments. The following description is presented to enable any person skilled in the art to make and use the invention. In the following description, details are set forth for the purpose of explanation. It will be apparent to one of ordinary skill in the art that the present invention may be practiced without these specific details. In other instances, well-known structures and processes are not shown in detail to avoid obscuring the description of the invention with unnecessary detail. Thus, the present invention is not intended to be limited to the embodiments shown, but is to be accorded the widest scope consistent with the principles disclosed herein.
Many technical difficulties are faced in the development of AlGaN-based ultraviolet LEDs, for example, electrons have small effective mass and high mobility, so that many electrons easily overflow to a P layer through a quantum well; with the increase of Al component, the problems of high defect density, uneven surface and the like of an epitaxially grown AlGaN film are easily caused, and it is difficult to obtain an AlGaN material with high crystal quality, and compared with a GaN material, the AlGaN material with high Al component is more difficult no matter N type doping or P type doping, especially the doping of P-AlGaN is troublesome, the activation efficiency of dopant Mg is low, so that the hole is insufficient, and the radiation recombination efficiency is reduced; in addition, the quantum efficiency in the AlGaN-based ultraviolet LED is lower than that of a blue-green light emitting diode, and the performance of the ultraviolet light emitting diode is severely limited. In order to improve the quantum efficiency of the ultraviolet LED, it is necessary to prepare p-type and n-type AlGaN materials with high conductivity, as well as epitaxial layers with high crystal quality and quantum well structures with high internal quantum efficiency.
At present, the quantum efficiency in the AlGaN-based ultraviolet LED is lower than that of a blue-green light emitting diode, and due to the serious pre-reaction of Al and NH3, the growth of the AlGaN material needs a lower V/III ratio (the molar ratio of V-valence atoms to III-valence atoms, such as the molar ratio of N to Ga), so that N vacancy occurs in an AlGaN epitaxial layer, the crystal quality of the epitaxial layer grown by the AlGaN material is lower than that of GaN, and the luminous efficiency of the ultraviolet LED is reduced. In addition, oxygen atoms decomposed at high temperature from the oxide on the surface of the substrate 1 may diffuse upward with the growth of the epitaxial layer, and also the crystal quality of the epitaxial layer may be reduced, so that the light emitting efficiency of the ultraviolet LED may be decreased.
The main body of the embodiment is a light emitting diode epitaxial wafer, which comprises a substrate 1, a buffer layer 2 and a first AlGaN layer, wherein a plasma processing layer 5 is deposited on the first AlGaN layer, and a multi-quantum well layer 6, an electron blocking layer 7 and a second AlGaN layer are sequentially grown on the plasma processing layer 5; the surface of the first AlGaN layer is provided with an N vacancy defect state surface layer, and the plasma processing layer 5 is used for reacting with the N vacancy defect state surface layer to grow a GaN film with higher quality. By carrying out plasma treatment on the first AlGaN layer, the plasma can react with the N vacancy defect state surface layer on the surface of the first AlGaN layer to form a plasma treatment layer with high crystal quality and stable structure, so that the problem of poor quality of the N vacancy defect state surface layer on the original first AlGaN layer is solved, the crystal quality of an epitaxial layer is further improved, and the luminous efficiency is further improved; meanwhile, in the plasma treatment process, oxygen atoms diffused on the substrate can be adsorbed by the active plasma, so that the content of the oxygen atoms on the first AlGaN layer is reduced, the oxygen atoms are prevented from extending and diffusing into the multiple quantum well layer, and the luminous efficiency is further improved.
More specifically, the substrate 1 may not include the buffer layer 2, or may be provided with other structural layers, as long as the AlGaN layer is provided with the plasma treatment layer 5, and the plasma treatment layer also plays a role in filling in N vacancy defects, or a role in adsorbing oxygen atoms diffused in the bottom layer, which are technical solutions of protection in this embodiment.
In some embodiments of the present application, the plasma processing layer 5 is sputtered on the first AlGaN layer by introducing plasma, and the plasma is N2And (4) O plasma. The same can also be used, and other plasmas capable of filling N vacancy defects can be used for processing, and are not limited to only N2O plasma, e.g. N2Plasma is generated. More specifically, other nitrogen-containing plasmas capable of absorbing and blocking oxygen atoms can be selected for processing, and the effect of improving the luminous efficiency of the LED is achieved.
In some embodiments of the present application, the first AlGaN layer includes an undoped AlGaN layer 3 and an N-type doped AlGaN layer 4 which are sequentially grown on the buffer layer 2, and the plasma treatment layer 5 is grown on the surface of the N-type doped AlGaN layer 4. The N-type doped AlGaN layer 4 is doped with Si with the thickness of 1.0-3.0 microns, the growth temperature of 1100-1200 ℃, the pressure of 50-100 Torr and the Si doping concentration of 1019cm-3-1020cm-3And the Al component is between 20 and 60 percent. The undoped AlGaN layer 3 grows at a temperature of 1000 ℃ to 1200 ℃, at a pressure range of 150Torr to 500Torr, and for a period of 5 minutes to 10 minutes.
In some embodiments of the present application, the second AlGaN layer comprises a P-type doped AlGaN layer, a contact layer 9 is disposed on a surface of the P-type doped AlGaN layer, and the contact layer 9 comprises an AlGaN structure. The thickness is between 10nm and 50nm, the growth temperature range is 1000 ℃ to 1100 ℃, the growth pressure range is 50Torr to 100Torr, and the Al component is between 0 percent and 30 percent.
Referring to fig. 1, the light emitting diode epitaxial wafer of the present embodiment includes a substrate 1, a buffer layer 2, an undoped AlGaN layer 3, an N-type doped AlGaN layer 4, a plasma processing layer 5, a multi-quantum well layer 6(MQW), an electron blocking layer 7(EBL), a P-type doped GaN layer 8, and a contact layer 9, which are sequentially disposed. Oxygen atoms on the substrate 1 can diffuse upwards along the buffer layer 2, the undoped AlGaN layer 3 and the N-type doped AlGaN layer 4, and if the oxygen atoms diffuse to the multiple quantum well layer 6, carriers of the multiple quantum well layer 6 can be absorbed, so that the luminous efficiency of the LED can be reduced; by arranging the plasma treatment layer 5 in front of the multiple quantum well layer 6, oxygen atoms which are about to enter the multiple quantum well layer 6 are intercepted by adsorbing the oxygen atoms through plasma on the plasma treatment layer 5, and the radiation recombination efficiency of carriers in the multiple quantum well layer 6 is further improved. Meanwhile, as the N-type doped AlGaN layer 4 has N vacancy defects during growth and affects the appearance of the multiple quantum well layer 6, the N vacancy defects of the N-type doped AlGaN layer 4 can be compensated by arranging the plasma processing layer 5, and the crystal quality of the epitaxial layer is improved.
By N-doping an AlGaN layer2Due to the fact that pre-reaction of Al and NH3 is serious, growth of AlGaN materials needs low V/III ratio conditions, N vacancies occur in AlGaN epitaxial layers, the crystal quality of the epitaxial layers is poor, and the luminous efficiency of the ultraviolet LED is reduced. The substrate with the grown epitaxial layer is positioned at the negative electrode of a power supply of a magnetron sputtering system, and N is carried out on the substrate2O plasma treatment, N2N atoms in the O plasma carry positive charges, move towards the epitaxial layer positioned at the negative electrode under the action of an electric field, and are combined with Ga atoms in an N vacancy defect state in the epitaxial layer to generate a GaN film, so that the crystal quality of the AlGaN epitaxial layer is improved; in addition, oxygen atoms can be decomposed from the oxide on the surface of the substrate in the epitaxial process and can be diffused upwards along with the growth of the epitaxial layer, and when the oxygen atoms are diffused to the quantum well layer, carriers can be absorbed to a certain extent, so that the radiation recombination efficiency of the carriers in the quantum well is reduced, and the luminous efficiency of the ultraviolet LED is reduced. By N2Treating with O plasma, decomposing oxygen atom with negative charge in the oxide on the surface of the substrate, and applying the oxygen atom with negative charge to N on the positive electrode under the action of electric field2O plasma movement, with N2Oxygen atoms in the O plasma are combined with generated oxygen molecules, so that the oxygen atoms are prevented from diffusing into the quantum well, and the luminous efficiency of the ultraviolet LED can be improved.
The main body of the embodiment is a method for preparing an epitaxial wafer of a light emitting diode, which comprises the following steps: providing a substrate 1; preparing a buffer layer 2 on a substrate 1, and then preparing a first AlGaN layer on the buffer layer 2; preparing a plasma processing layer 5 on the first AlGaN layer to make up for N vacancy defects on the first AlGaN layer; and sequentially growing a multi-quantum well layer 6, an electron blocking layer 7 and a second AlGaN layer on the plasma processing layer 5.
In some embodiments of the present application, the step of preparing the plasma treatment layer 5 includes introducing N2And O plasma is prepared by adopting a radio frequency controlled sputtering method. In some embodiments of the present application, in the step of preparing the first AlGaN layer, the method further includes the steps of: growing an undoped AlGaN layer 3 on the buffer layer 2 at a high temperature; an N-type doped AlGaN layer 4 grows on the undoped AlGaN layer 3, and the N-type doped AlGaN layer 4 is doped with Si. In some embodiments of the present application, the step of preparing the second AlGaN layer includes growing a P-type doped AlGaN layer on the electron blocking layer 7, and the P-type doping is Mg doping.
Referring to fig. 2, in some embodiments of the present application, the method includes the following steps: s1: providing a sapphire Al2O3 substrate 1; s2: growing a buffer layer 2 on a substrate 1 by adopting a physical vapor deposition method, and carrying out in-situ annealing treatment on the buffer layer 2; s3: after the annealing is finished, growing an undoped AlGaN layer 3 on the buffer layer 2 at a high temperature, wherein the Al component is between 30 and 80 percent; s4: growing a Si-doped N-type doped AlGaN layer 4 on the undoped AlGaN layer 3, wherein the Al component is between 20 and 60 percent; s5: introducing N on the N-type doped AlGaN layer 42O plasma, preparing a plasma treatment layer 5 by adopting a radio frequency controlled sputtering method; s6: preparing a multi-quantum well layer 6 on the plasma processing layer 5 by an MOCVD method, wherein the multi-quantum well layer 6 is GaN/AlGaN with 5 to 12 periods, GaN is a well layer, and AlGaN is a barrier layer; s7: growing an AlGaN electronic barrier layer 7 on the multi-quantum well layer 6; s8: a P-type doped GaN layer 8 is grown on the electron blocking layer 7, and the doping element is Mg. S9: and growing an AlGaN contact layer 9 on the P-type doped GaN layer 8, and annealing the whole epitaxial structure after the contact layer 9 is prepared.
Example 1: the embodiment provides an epitaxial preparation method of an AlGaN-based ultraviolet light-emitting diode. A substrate 1 made of sapphire Al in (0001) crystal orientation2O3Is a substrate 1.
Step 1: an AlN buffer layer 2 is grown on a substrate 1 using PVD. The growth temperature is 400-650 ℃, the sputtering power is 2000-4000W, and the pressure is 1-10 torr; an AlN buffer layer 2 of 15 to 50nm thickness was grown.
Step 2: the buffer layer 2 is subjected to in-situ annealing treatment in MOCVD in a hydrogen atmosphere at a temperature of 1000 ℃ to 1200 ℃, at a pressure range of 150Torr to 500Torr for a period of 5 minutes to 10 minutes.
And step 3: after the annealing is finished, the temperature is adjusted to 1050 ℃ -1200 ℃, undoped AlGaN with the thickness of 1.0-3.0 microns is grown, the growth pressure is 50Torr-100Torr, and the Al component is 0.3-0.8.
And 4, step 4: after the growth of the undoped AlGaN layer is finished, a Si-doped N-type AlGaN layer grows, the thickness of the Si-doped N-type AlGaN layer is 1.0-3.0 microns, the growth temperature is 1100-1200 ℃, the pressure is 50Torr-100Torr, and the Si doping concentration is 1019cm-3-1020cm-3And the Al component is between 0.2 and 0.6.
And 5: after the growth of the N-type doped AlGaN layer 4 is finished, the temperature is reduced to room temperature and the N-type doped AlGaN layer is transferred into a radio frequency magnetron sputtering system, and N2The O plasma is positioned at the anode of a power supply of the magnetron sputtering system, the substrate on which the epitaxial layer grows is positioned at the cathode of the power supply of the magnetron sputtering system, and N is carried out on the substrate2O plasma treatment for 30-60min with sputtering power of 100-2The flow rate of O is 20-50sccm, the temperature is 100-.
Step 6: n is a radical of2Continuing to transfer the substrate into MOCVD to grow a multi-quantum well structure (MQW) after O plasma treatment is finished, wherein the multi-quantum well layer 6(MQW) is composed of 5-12 periods of GaN/AlGaN, wherein GaN is a well layer, AlGaN is a barrier layer, the thickness of a single GaN well layer in the MQW is 2-4nm, the growth temperature range is 900-1000 ℃, and the pressure range is between 50Torr and 200 Torr; the thickness of the single AlGaN barrier layer is between 8 and 20nm, the growth temperature is between 1000 and 1100 ℃, the growth pressure is between 50 and 100Torr, and the Al component is between 0.1 and 0.5.
And 7: after the multi-quantum well layer 6 grows, the AlGaN electronic barrier layer 7EBL26 grows at the temperature of between 1000 and 1100 ℃, the growth pressure of between 50 and 100Torr, the growth thickness of between 20 and 100nm and the Al component of between 0.1 and 0.5.
And 8: after the electron blocking layer 7EBL grows, a P-type doped GaN layer 8 grows,the thickness is between 30nm and 200nm, the growth temperature is between 950 ℃ and 1050 ℃, the growth pressure interval is between 50Torr and 300Torr, the Mg doping concentration is 1019cm-3-1020cm-3In the meantime.
And step 9: AlGaN contact is grown on the P-type doped GaN layer 8, the thickness is between 10nm and 50nm, the growth temperature interval is 1000-1100 ℃, the growth pressure interval is 50-100 Torr, and the Al component is between 0.0-0.3.
Step 10: and after the epitaxial structure growth is finished, reducing the temperature of the reaction cavity, annealing in a nitrogen atmosphere, wherein the annealing temperature range is 650-850 ℃, annealing for 5-15 minutes, and finishing the epitaxial growth at room temperature.
In this example, trimethylaluminum (TMAl), trimethylgallium or triethylgallium (TMGa or TEGa), NH3 were used as precursors for group III and group V sources, respectively, silane and dimocene as precursors for N-and P-type dopants, respectively, N2And H2As a carrier gas.
In the above embodiments, the descriptions of the respective embodiments have respective emphasis, and parts that are not described in detail in a certain embodiment may refer to the above detailed descriptions of other embodiments, and are not described herein again.
Having thus described the basic concept, it will be apparent to those skilled in the art that the foregoing detailed disclosure is to be considered merely illustrative and not restrictive of the broad application. Various modifications, improvements and adaptations to the present application may occur to those skilled in the art, although not explicitly described herein. Such modifications, improvements and adaptations are proposed in the present application and thus fall within the spirit and scope of the exemplary embodiments of the present application.
Also, this application uses specific language to describe embodiments of the application. Reference throughout this specification to "one embodiment," "an embodiment," and/or "some embodiments" means that a particular feature, structure, or characteristic described in connection with at least one embodiment of the present application is included in at least one embodiment of the present application. Therefore, it is emphasized and should be appreciated that two or more references to "an embodiment" or "one embodiment" or "an alternative embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, some features, structures, or characteristics of one or more embodiments of the present application may be combined as appropriate.
Similarly, it should be noted that in the preceding description of embodiments of the application, various features are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the disclosure aiding in the understanding of one or more of the embodiments. This method of disclosure, however, is not intended to require more features than are expressly recited in the claims. Indeed, the embodiments may be characterized as having less than all of the features of a single embodiment disclosed above.
Numerals describing the number of components, attributes, etc. are used in some embodiments, it being understood that such numerals used in the description of the embodiments are modified in some instances by the use of the modifier "about", "approximately" or "substantially". Unless otherwise indicated, "about", "approximately" or "substantially" indicates that the number allows a variation of ± 20%. Accordingly, in some embodiments, the numerical parameters used in the specification and claims are approximations that may vary depending upon the desired properties of the individual embodiments. In some embodiments, the numerical parameter should take into account the specified significant digits and employ a general digit preserving approach. Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the range are approximations, in the specific examples, such numerical values are set forth as precisely as possible within the scope of the application.
For each patent, patent application publication, and other material cited in this application, such as articles, books, specifications, publications, documents, and the like, the entire contents of which are hereby incorporated by reference into this application, except for application history documents that are inconsistent with or conflict with the contents of this application, and except for documents that are currently or later become incorporated into this application as though fully set forth in the claims below. It is noted that the descriptions, definitions and/or use of terms in this application shall control if they are inconsistent or contrary to the present disclosure.
The technical solutions provided by the embodiments of the present application are described in detail above, and the principles and embodiments of the present invention are explained herein by using specific examples, and the descriptions of the above embodiments are only used to help understanding the method and the core ideas of the present invention; meanwhile, for those skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. The light-emitting diode epitaxial wafer is characterized by comprising a substrate and a laminated structure arranged on the substrate, wherein the laminated structure at least comprises a first AlGaN layer and a multi-quantum well layer which are arranged from bottom to top, one side, close to the multi-quantum well layer, of the first AlGaN layer is provided with a plasma treatment layer, the plasma treatment layer is made by the reaction of a surface layer of the first AlGaN layer and plasma, and the surface layer is an N-vacancy defect state surface layer.
2. The light-emitting diode epitaxial wafer according to claim 1, wherein the plasma is a nitrogen-containing plasma, and the plasma treatment layer is a GaN thin film.
3. The light-emitting diode epitaxial wafer according to claim 1, wherein the first AlGaN layer comprises an undoped AlGaN layer and an N-type doped AlGaN layer from bottom to top in sequence, and the plasma treatment layer is grown on the side of the N-type doped AlGaN layer far away from the undoped AlGaN layer.
4. The light-emitting diode epitaxial wafer as claimed in claim 3, wherein the N-type doped AlGaN layer comprises an N-vacancy defect state surface layer, and the plasma treatment layer is formed by reacting the plasma with the N-vacancy defect state surface layer.
5. The light emitting diode epitaxial wafer of claim 1, wherein the light emitting diode epitaxial wafer is characterized in thatIn that the plasma is N2And (4) O plasma.
6. A preparation method of a light emitting diode epitaxial wafer is characterized by comprising the following steps:
providing a substrate;
preparing a laminated structure on a substrate, wherein the laminated structure at least comprises a first AlGaN layer and a multi-quantum well layer which are arranged from bottom to top;
after the first AlGaN layer is prepared, carrying out plasma treatment on one side, close to the multi-quantum well layer, of the first AlGaN layer to form a plasma treatment layer;
the plasma processing step comprises the step of reacting plasma with the N-vacancy defect state surface layer of the first AlGaN layer to generate a plasma processing layer.
7. The method for preparing an epitaxial wafer for light-emitting diodes according to claim 6, wherein in the step of preparing the first AlGaN layer, the method further comprises the steps of:
growing an undoped AlGaN layer at a high temperature;
and growing an N-type doped AlGaN layer on the undoped AlGaN layer, wherein the N-type doped AlGaN layer is doped with Si.
8. The method for preparing an epitaxial wafer for light-emitting diodes according to claim 7, wherein the step of preparing the plasma treatment layer comprises placing the substrate on which the N-type doped AlGaN layer has been grown at a negative electrode position in a magnetron sputtering system, introducing a plasma containing nitrogen plasma at a positive electrode position in the system, and reacting the plasma with an N-vacancy defect state surface layer of the N-type doped AlGaN layer to form a GaN film.
9. The method for preparing the light-emitting diode epitaxial wafer as claimed in claim 6, characterized by comprising the following steps:
providing a sapphire Al2O3A substrate;
growing a buffer layer on the substrate by adopting a physical vapor deposition method, and carrying out in-situ annealing treatment on the buffer layer;
after the annealing is finished, growing an undoped AlGaN layer on the buffer layer at a high temperature, wherein the Al component is between 30 and 80 percent;
growing a Si-doped N-type doped AlGaN layer on the undoped AlGaN layer, wherein the Al component is between 20 and 60 percent;
introducing N on the N-type doped AlGaN layer2O plasma, preparing a plasma treatment layer by adopting a radio frequency controlled sputtering method;
preparing a multi-quantum well layer on the plasma processing layer by an MOCVD method, wherein the multi-quantum well layer is GaN/AlGaN with 5 to 12 periods, GaN is a well layer, and AlGaN is a barrier layer;
growing an AlGaN electronic barrier layer on the multi-quantum well layer;
and growing a P-type doped GaN layer on the electron blocking layer, wherein the doping element is Mg.
10. The method for preparing the epitaxial wafer of the light-emitting diode according to claim 9, further comprising growing an AlGaN contact layer on the P-type doped GaN layer, and annealing the whole epitaxial structure after the contact layer is prepared.
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