CN116885069A - Light extraction layer, ultraviolet LED epitaxial structure, and preparation method and application thereof - Google Patents
Light extraction layer, ultraviolet LED epitaxial structure, and preparation method and application thereof Download PDFInfo
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
- H01L33/20—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 particular shape, e.g. curved or truncated substrate
- H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
- H01L33/12—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 stress relaxation structure, e.g. buffer layer
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/44—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 coatings, e.g. passivation layer or anti-reflective coating
- H01L33/46—Reflective coating, e.g. dielectric Bragg reflector
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to the technical field of ultraviolet LED epitaxial structures, and particularly relates to a light extraction layer, a preparation method and application thereof, an ultraviolet LED epitaxial structure and a preparation method thereof. The light extraction layer provided by the invention comprises an undoped AlGaN layer and a P-type AlGaN covering layer which are sequentially stacked from bottom to top; the undoped AlGaN layer is provided with a hexagonal defect pit filled with reflective metal; the upper surface of the hexagonal defect pit filled with the reflective metal is in contact with the P-type AlGaN cladding layer. According to the invention, by corroding the undoped AlGaN layer, a plurality of hexagonal defect pits can be generated, and besides the dislocation on the surface is outdated, the stress in the growth process can be released through secondary epitaxy in the subsequent growth, so that the crystal quality of an epitaxial structure is improved; according to the invention, the high-reflection metal layer is deposited in the defect pit, so that the reflection of light in the epitaxial layer can be increased, and the light extraction efficiency is greatly improved.
Description
Technical Field
The invention belongs to the technical field of ultraviolet LED epitaxial structures, and particularly relates to a light extraction layer, a preparation method and application thereof, an ultraviolet LED epitaxial structure and a preparation method thereof.
Background
Ultraviolet rays can destroy DNA or RNA molecular structure in bacterial virus, and can remove H 3 N 2 Influenza virus, E.coli, golden yellowStaphylococci and the like are tens of common viruses and bacteria, so the staphylococci are often used as sterilizing light sources for water and air in public places such as airports, hospitals, stations and the like and household appliances. At present, the AlGaN-based ultraviolet LED can realize luminescence within a spectrum range of 200 nm-365 nm by changing the doping amount of the Al element in an active region, has excellent performances of stable physicochemical property, high temperature resistance, radiation resistance and the like, and is an ideal choice for next-generation ultraviolet light sources.
Although the application prospect of ultraviolet LEDs is wide, compared with blue light, the ultraviolet LEDs still face a plurality of difficulties to be solved, and the core is low luminous efficiency and light extraction efficiency, which severely restricts the further application of the ultraviolet LEDs. Currently, ultraviolet LEDs are generally heteroepitaxially grown, and during heteroepitaxial growth, significant internal stress accumulation is easily formed due to mismatch and grain fusion, and release is performed to a certain extent through dislocation and crack forms, which makes the dislocation density of the ultraviolet LED high to 108cm -2 Magnitude. Particularly, in the P-type heterogeneous epitaxy with high Al component, larger dislocation density is easier to generate due to larger lattice mismatch, the defects can greatly reduce the crystal quality of the P-type epitaxial layer, larger leakage channels and non-radiative recombination centers are generated, and the luminous efficiency of the device is seriously reduced. Meanwhile, because the Mg doping of the high Al component is difficult at present, the bulk resistance of the P-type epitaxial layer is often larger, and a thicker P-type GaN layer is often grown for forming better ohmic contact with the chip metal electrode. However, since the forbidden bandwidth of GaN is smaller than that of AlGaN material, serious light absorption occurs, resulting in lower light extraction efficiency of AlGaN-based uv LED epitaxial structure.
Disclosure of Invention
The invention aims to provide a light extraction layer, a preparation method and application thereof, an ultraviolet LED epitaxial structure and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a light extraction layer, which comprises an undoped AlGaN layer and a P-type AlGaN covering layer which are sequentially stacked from bottom to top;
the undoped AlGaN layer is provided with a hexagonal defect pit filled with reflective metal; the upper surface of the hexagonal defect pit filled with the reflective metal is in contact with the P-type AlGaN cladding layer.
Preferably, the thickness of the undoped AlGaN layer is 10-20 nm;
the thickness of the P-type AlGaN coating layer is 30-50 nm.
Preferably, the reflective metal comprises one or more of Ag, al, pt, fe and Pd.
The invention also provides a preparation method of the light extraction layer, which comprises the following steps:
growing an undoped AlGaN layer on the surface of the substrate;
etching the surface of the undoped AlGaN layer to obtain a hexagonal defect pit;
and after depositing reflective metal in the hexagonal defect pits, growing a P-type AlGaN covering layer on the surface of the undoped AlGaN layer to obtain the light extraction layer.
Preferably, the growth modes of the undoped AlGaN layer and the P-type AlGaN covering layer are organic metal chemical vapor deposition;
the growth conditions of the undoped AlGaN layer include: the reaction pressure is 20-30 mabr, and the reaction temperature is 1100-1150 ℃;
the growth conditions of the P-type AlGaN coating layer comprise: the reaction pressure is 20-30 mabr, and the reaction temperature is 1100-1150 ℃.
Preferably, the corrosive agent adopted by the corrosion comprises KOH aqueous solution or NaOH aqueous solution;
the conditions for depositing the reflective metal include: working pressure of 1.0X10 -6 ~4.0×10 -6 The Torr, the output power of the electron gun is 3-4 kW, and the coating power is 0.3-0.4 times of the output power of the electron gun.
The invention also provides an application of the light extraction layer prepared by the technical scheme or the preparation method of the technical scheme in an ultraviolet LED epitaxial structure.
The invention also provides an ultraviolet LED epitaxial structure which comprises a substrate, an AlN buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a multiple quantum well layer, an electron blocking layer, a hole injection layer, a light extraction layer and a P-type GaN layer which are sequentially stacked;
the light extraction layer is the light extraction layer prepared by the technical scheme or the preparation method;
and the undoped AlGaN layer in the light extraction layer is contacted with the hole injection layer, and the P-type AlGaN covering layer is contacted with the P-type GaN layer.
Preferably, the thickness of the AlN buffer layer is 4-6 μm;
the thickness of the undoped AlGaN layer is 2-3 mu m;
the thickness of the N-type AlGaN layer is 1-2 mu m;
the multi-quantum well layer comprises a quantum well light-emitting layer and a quantum barrier layer which are alternately stacked; the number of periods of the alternate lamination is 5; in a single period, the thickness of the quantum well light-emitting layer is 2.5nm, and the thickness of the quantum barrier layer is 13nm;
the thickness of the electron blocking layer is 30-50 nm;
the thickness of the hole injection layer is 20-30 nm;
the thickness of the P-type GaN layer is 150-300 nm.
The invention also provides a preparation method of the ultraviolet LED epitaxial structure, which comprises the following steps:
and sequentially growing an AlN buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a multi-quantum well layer, an electron blocking layer, a hole injection layer, a light extraction layer and a P-type GaN layer on the surface of the substrate, and annealing to obtain the ultraviolet LED epitaxial structure.
The invention provides a light extraction layer, which comprises an undoped AlGaN layer and a P-type AlGaN covering layer which are sequentially stacked from bottom to top; the undoped AlGaN layer is provided with a hexagonal defect pit filled with reflective metal; the upper surface of the hexagonal defect pit filled with the reflective metal is in contact with the P-type AlGaN cladding layer. According to the invention, by corroding the undoped AlGaN layer, special hexagonal defect pits are generated on the surface of the undoped AlGaN layer, and the obtained hexagonal defect pits not only enable dislocation on the surface to leak out, but also release stress in the growth process through secondary epitaxy in subsequent growth, so that the crystal quality of an epitaxial structure is improved; in addition, due to the existence of the P-type GaN layer, excessive light emitted from the active layer is lost in the epitaxial layer, so that the light extraction efficiency is low, and the light emitting efficiency of the LED chip is low; according to the invention, the high-reflection metal layer is deposited in the defect pit, so that the reflection of light in the epitaxial layer can be increased, and the light extraction efficiency is greatly improved.
Drawings
FIG. 1 is a schematic cross-sectional view of a light extraction layer when the bottom surface of a hexagonal defect pit is tapered;
FIG. 2 is a schematic cross-sectional view of a light extraction layer when the bottom surface of a hexagonal defect pit is planar;
fig. 3 is a schematic cross-sectional view of a light extraction layer when the bottom surface of a hexagonal defect pit has both a taper and a land.
Detailed Description
The invention provides a light extraction layer, which comprises an undoped AlGaN layer and a P-type AlGaN covering layer which are sequentially stacked from bottom to top;
the undoped AlGaN layer is provided with a hexagonal defect pit filled with reflective metal; the upper surface of the hexagonal defect pit filled with the reflective metal is in contact with the P-type AlGaN cladding layer.
In the present invention, the thickness of the undoped AlGaN layer is preferably 10 to 20nm, more preferably 12 to 18nm, and even more preferably 15 to 16nm. In the invention, the material of the undoped AlGaN layer is preferably Al 0.45 Ga 0.55 N。
In the present invention, the thickness of the P-type AlGaN cladding layer is preferably 30 to 50nm, more preferably 35 to 48nm, and even more preferably 40 to 45nm. In the invention, the material of the P-type AlGaN coating layer is preferably Al 0.4 Ga 0.6 N; the P-type AlGaN cladding layer is also preferably doped with magnesium, and the doping concentration of the magnesium is preferably 1.6x10 19 cm -3 。
In the present invention, the bottom surface of the hexagonal defect pit is preferably tapered and/or planar. In the present invention, a schematic cross-sectional view of the light extraction layer when the bottom surface of the hexagonal defect pit is tapered is shown in fig. 1; a schematic cross-sectional view of the light extraction layer when the bottom surface of the hexagonal defect pit is planar is shown in fig. 2; a schematic cross-sectional view of the light extraction layer when the bottom surface of the hexagonal defect pit has both a taper and a land is shown in FIG. 3. The present invention is not particularly limited to the size of the hexagonal defect pits, and may be employed as is well known to those skilled in the art.
In the present invention, the reflective metal preferably includes one or more of Ag, al, pt, fe and Pd. The present invention is not particularly limited in the amount of the reflective metal and the number of the defect pits, and those skilled in the art can be used.
The invention also provides a preparation method of the light extraction layer, which comprises the following steps:
growing an undoped AlGaN layer on the surface of the substrate;
etching the surface of the undoped AlGaN layer to obtain a hexagonal defect pit;
and after depositing reflective metal in the hexagonal defect pits, growing a P-type AlGaN covering layer on the surface of the undoped AlGaN layer to obtain the light extraction layer.
The invention grows an undoped AlGaN layer on the surface of the substrate.
The kind of the substrate is not particularly limited, and those skilled in the art can be used.
In the invention, the growth mode of the undoped AlGaN layer is preferably organic metal chemical vapor deposition; the growth conditions of the undoped AlGaN layer preferably include: the reaction pressure is 20-30 mabr, and the reaction temperature is 1100-1150 ℃.
In the present invention, the growth of the undoped AlGaN layer preferably includes: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity 3 And growing an undoped AlGaN layer on the surface of the substrate.
After the undoped AlGaN layer is obtained, the surface of the undoped AlGaN layer is corroded to obtain the hexagonal defect pit.
In the present invention, the etchant used for the etching preferably includes an aqueous KOH solution or an aqueous NaOH solution. In the present invention, the mass concentration of the KOH aqueous solution is preferably 50%; the mass concentration of the aqueous NaOH solution is preferably 50%. In the invention, the temperature of the corrosion is preferably 30-60 ℃ and the time is preferably 10-15 min.
After the corrosion, the invention also preferably comprises the steps of flushing and drying the obtained matrix with nitrogen; the flushing process is preferably as follows: and washing by adopting dilute hydrochloric acid, acetone, absolute ethyl alcohol and deionized water in turn. In the invention, residual corrosive agent on the surface can be washed away by washing with dilute hydrochloric acid, so that continuous corrosion is prevented; the surface oxide and impurities can be washed off by washing with acetone, absolute ethyl alcohol and deionized water.
After the hexagonal defect pits are obtained, the light extraction layer is obtained by depositing reflective metal in the hexagonal defect pits and then growing a P-type AlGaN covering layer on the surface of the undoped AlGaN layer.
In the present invention, the conditions for depositing the reflective metal preferably include: working pressure of 1.0X10 -6 ~4.0×10 -6 The Torr, the output power of the electron gun is 3-4 kW, and the coating power is 0.3-0.4 times of the output power of the electron gun. In the invention, the output power of the electron gun is the coating speed. In the invention, the target material used for depositing the reflective metal is preferably a metal simple substance with the purity of more than or equal to 99.99 percent, and the type of the metal simple substance corresponds to the type of the reflective metal.
After the depositing the reflective metal, the invention also preferably comprises removing the reflective metal in the pit area without the hexagonal defect; the removal is preferably plasma etching. The plasma etching process is not particularly limited, and the method is well known to those skilled in the art; the plasma etching is preferably performed in an ICP plasma etcher.
In the invention, the growth mode of the P-type AlGaN covering layer is preferably organic metal chemical vapor deposition; the growth conditions of the P-type AlGaN cladding layer preferably comprise: the reaction pressure is 20-30 mabr, and the reaction temperature is 1100-1150 ℃.
In the present invention, the growth of the P-type AlGaN cladding layer preferably includes: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity 3 And a magnesium-cyclopentadienyl (Cp 2 Mg) layer, wherein a P-type AlGaN covering layer is grown on the surface of the undoped AlGaN layer.
The invention also provides an application of the light extraction layer prepared by the technical scheme or the preparation method of the technical scheme in an ultraviolet LED epitaxial structure.
The invention also provides an ultraviolet LED epitaxial structure which comprises a substrate, an AlN buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a multiple quantum well layer, an electron blocking layer, a hole injection layer, a light extraction layer and a P-type GaN layer which are sequentially stacked;
the light extraction layer is the light extraction layer prepared by the technical scheme or the preparation method;
and the undoped AlGaN layer in the light extraction layer is contacted with the hole injection layer, and the P-type AlGaN covering layer is contacted with the P-type GaN layer.
In the present invention, the substrate is preferably sapphire; in a specific embodiment, the sapphire is preferably 2 inches in size.
In the present invention, the thickness of the AlN buffer layer is preferably 4 to 6. Mu.m, more preferably 4 to 5. Mu.m.
In the invention, the thickness of the undoped AlGaN layer is preferably 2-3 μm; the material of the undoped AlGaN layer is preferably Al 0.7 Ga 0.3 N。
In the invention, the thickness of the N-type AlGaN layer is preferably 1-2 μm; the material of the N-type AlGaN layer is preferably Al 0.55 Ga 0.45 N; the N-type AlGaN layer is also preferably doped with silicon; the doping concentration of the silicon is preferably 5 x 10 18 cm -3 。
In the invention, the multiple quantum well layer is excellentThe quantum well light-emitting layer and the quantum barrier layer are alternately stacked; the number of cycles of the alternate lamination is preferably 5; in a single cycle, the thickness of the quantum well light emitting layer is preferably 2.5nm, and the thickness of the quantum barrier layer is preferably 13nm. In the present invention, the material of the quantum well light-emitting layer is preferably Al 0.55 Ga 0.45 N or Al 0.42 Ga 0.58 N; the material of the quantum barrier layer is preferably Al 0.55 Ga 0.45 N or Al 0.42 Ga 0.58 N; the quantum barrier layer is also preferably doped with silicon; the doping concentration of the silicon is preferably 3 x 10 18 cm -3 . In the present invention, the quantum well light emitting layer is in contact with the N-type AlGaN layer, and the quantum barrier layer is in contact with the electron blocking layer.
In the invention, the thickness of the electron blocking layer is preferably 30-50 nm, more preferably 35-45 nm, and even more preferably 40nm; the material of the electron blocking layer is preferably Al 0.75 Ga 0.25 N; the electron blocking layer is also preferably doped with magnesium; the doping concentration of the magnesium is preferably 1 x 10 19 cm -3 。
In the invention, the thickness of the hole injection layer is preferably 20-30 nm, more preferably 22-28 nm, and even more preferably 25-26 nm; the material of the hole injection layer is preferably Al 0.45 Ga 0.55 N; the hole injection layer is also preferably doped with magnesium; the doping concentration of the magnesium is preferably 1.5×10 19 cm -3 。
In the invention, the thickness of the P-type GaN layer is preferably 150-300 nm, more preferably 200-250 nm, and even more preferably 220-230 nm; the P-type GaN layer is also preferably doped with magnesium; the doping concentration of the magnesium is preferably 1 x 10 20 cm -3 。
The invention also provides a preparation method of the ultraviolet LED epitaxial structure, which comprises the following steps:
and sequentially growing an AlN buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a multi-quantum well layer, an electron blocking layer, a hole injection layer, a light extraction layer and a P-type GaN layer on the surface of the substrate, and annealing to obtain the ultraviolet LED epitaxial structure.
In the present invention, all raw materials are commercially available products well known to those skilled in the art unless specified otherwise.
The invention also preferably includes pre-treating the substrate prior to growing; the reaction pressure of the pretreatment is preferably 30-50 mbar, the temperature is preferably 1000-1100 ℃, and the heat preservation time is preferably 5-10 min.
In the present invention, the growth mode is preferably organic metal chemical vapor deposition.
In the present invention, the growth of the AlN buffer layer preferably includes: introducing Trimethylaluminum (TMAL) and NH into the reaction cavity under the conditions that the reaction pressure is 30-50 mbar and the reaction temperature is 1200-1300 DEG C 3 And growing an AlN buffer layer on the surface of the substrate.
In the present invention, the growth of the undoped AlGaN layer preferably includes: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity under the conditions that the reaction pressure is 30-50 mbar and the reaction temperature is 1100-1200 DEG C 3 And growing an undoped AlGaN layer on the surface of the AlN buffer layer.
In the present invention, the growth of the N-type AlGaN layer preferably includes: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity under the conditions that the reaction pressure is 30-50 mbar and the reaction temperature is 1100-1150 DEG C 3 And SiH 4 And growing an N-type AlGaN layer on the surface of the undoped AlGaN layer.
In the present invention, the growth of the quantum well light emitting layer in the multiple quantum well layer preferably includes: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity under the conditions that the reaction pressure is 30-100 mbar and the reaction temperature is 1110-1150 DEG C 3 And growing the quantum well light-emitting layer. In the present invention, the growth of the quantum barrier layer in the multiple quantum well layer preferably includes: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity under the conditions that the reaction pressure is 30-100 mbar and the reaction temperature is 1110-1150 DEG C 3 And SiH 4 And growing the quantum barrier layer.
In the present invention, the electricityThe growth of the sub-barrier layer preferably comprises: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity under the conditions that the reaction pressure is 20-30 mbar and the reaction temperature is 1100-1150 DEG C 3 And a magnesium-cyclopentadienyl (Cp 2 Mg) layer, wherein an electron blocking layer is grown on the surface of the outermost quantum barrier layer of the multi-quantum well layer.
In the present invention, the growth of the hole injection layer preferably includes: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity under the conditions that the reaction pressure is 20-30 mbar and the reaction temperature is 1100-1150 DEG C 3 And a magnesium-cyclopentadienyl (Cp 2 Mg) layer, wherein a hole injection layer is grown on the surface of the electron blocking layer.
In the present invention, the preparation method of the light extraction layer is consistent with the method of the light extraction layer defined in the above technical solution, and will not be described herein.
In the present invention, the growth of the P-type GaN layer preferably includes: introducing trimethyl gallium (TMGa) and NH into the reaction cavity under the conditions that the reaction pressure is 100-400 mbar and the reaction temperature is 850-980 DEG C 3 And a magnesium cyclopentadienyl (Cp 2 Mg) layer, wherein a P-type GaN layer grows on the surface of the P-type AlGaN covering layer of the light extraction layer.
In the present invention, the annealing treatment conditions preferably include: the pressure is 20-30 mbar, the temperature is 750-850 ℃, and the heat preservation time is 30-50 min; the annealing treatment is preferably performed under a nitrogen atmosphere.
After the annealing treatment, the present invention also preferably includes furnace cooling the resulting epitaxial structure to room temperature.
For further explanation of the present invention, a light extraction layer, a method for preparing the same, an application thereof, an ultraviolet LED epitaxial structure, and a method for preparing the same, provided by the present invention, are described in detail below with reference to the accompanying drawings and examples, which should not be construed as limiting the scope of the present invention.
Example 1
Placing a 2-inch sapphire substrate on a carrying disc in a reaction cavity, and preprocessing for 10min under the conditions that the reaction pressure is 30mbar and the temperature is 1100 ℃;
at a reaction pressure of 30mbar and a reaction temperatureIntroducing Trimethylaluminum (TMAL) and NH into the reaction chamber at 1250 DEG C 3 Growing an AlN buffer layer with the thickness of 4 mu m on the surface of the sapphire substrate;
introducing trimethylgallium (TMGa), trimethylaluminum (TMAL) and NH into the reaction chamber under the conditions of a reaction pressure of 50mbar and a reaction temperature of 1180 DEG C 3 Growing an undoped AlGaN layer with the thickness of 3 mu m on the surface of the AlN buffer layer, wherein the AlGaN undoped layer is made of Al 0.7 Ga 0.3 N；
Introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction chamber under the conditions of reaction pressure of 50mbar and reaction temperature of 1150 DEG C 3 And SiH 4 Growing an N-type AlGaN layer with the thickness of 1.5 mu m on the surface of the undoped AlGaN layer, wherein the material of the N-type AlGaN layer is Al 0.55 Ga 0.45 The doping concentration of N and Si is 5 x 10 18 cm -3 ；
Alternately growing a quantum well light-emitting layer and a quantum barrier layer with 5 periods on the surface of the N-type AlGaN layer, wherein the growth process of the quantum well light-emitting layer in a single period is as follows: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction chamber under the conditions of reaction pressure of 30mbar and reaction temperature of 1110 DEG C 3 A quantum well light-emitting layer with a thickness of 2.5nm (wherein the material of the quantum well light-emitting layer is Al 0.42 Ga 0.58 N); the growth process of the quantum barrier layer is as follows: introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity under the conditions of reaction pressure of 30mbar and reaction temperature of 1110 DEG C 3 And SiH 4 A quantum barrier layer with a thickness of 13nm is grown (wherein the material of the quantum barrier layer is Al 0.55 Ga 0.45 The doping concentration of N and Si is 3 x 10 18 cm -3 ）；
Introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction cavity under the conditions of reaction pressure of 30mbar and reaction temperature of 1120 DEG C 3 And a magnesium-cyclopentadienyl (Cp 2 Mg) layer for growing an electron blocking layer with the thickness of 50nm on the surface of the quantum barrier layer, wherein the electron blocking layer is made of the following materialsAl 0.75 Ga 0.25 The doping concentration of N and Mg is 1 x 10 19 cm -3 ；
Introducing trimethylgallium (TMGa) Trimethylaluminum (TMAL) and NH into the reaction chamber under the conditions of reaction pressure of 30mbar and reaction temperature of 1100 DEG C 3 And a hole injection layer with a thickness of 20nm is grown by using magnesium dichloride (Cp 2 Mg), wherein the material of the hole injection layer is Al 0.45 Ga 0.55 The doping concentration of N and Mg is 1.5 x 10 19 cm -3 ；
Introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAL) and NH into the reaction chamber under the conditions of reaction pressure of 30mbar and reaction temperature of 1100 DEG C 3 Growing an undoped AlGaN layer with the thickness of 15nm on the surface of the hole injection layer, wherein the undoped AlGaN layer is made of Al 0.45 Ga 0.55 N；
After the growth of the undoped AlGaN layer is finished, taking out the epitaxial wafer, and putting the epitaxial wafer into a KOH aqueous solution with the temperature of 40 ℃ and the mass concentration of 50% to be corroded for 10min; washing with dilute hydrochloric acid to remove residual corrosive liquid on the surface, cleaning a sample with acetone, absolute ethyl alcohol and deionized water to remove oxides and impurities on the surface, and finally drying the surface with nitrogen to obtain a plurality of hexagonal defect pits;
placing the corroded epitaxial wafer into an electron beam vacuum coating reaction cavity, using a metal aluminum simple substance (the purity is more than or equal to 99.99%) as a target material, growing an aluminum simple substance on the surface of the undoped AlGaN layer, and filling the precipitated aluminum simple substance into a hexagonal defect pit, wherein the growth conditions for growing the aluminum simple substance comprise: the temperature of the cavity is 240 ℃, the output power of the electron gun is 3kW, the coating power is 1.05kW, and the pressure of the cavity is 4.0 x 10 -6 Torr; after the growth is completed, the obtained epitaxial wafer is put into ICP plasma etching equipment, and aluminum metal simple substance at the position without hexagonal defect pits on the surface of the undoped AlGaN layer is removed;
cleaning the epitaxial wafer, placing into a reaction chamber, introducing trimethyl gallium (TMGa), trimethyl aluminum (TMAl) NH3 and magnesium dichloride (Cp 2 Mg) into the reaction chamber under the conditions of reaction pressure of 30mbar and reaction temperature of 1100 ℃,growing an AlGaN covering layer with the thickness of 40nm on the surface of the undoped AlGaN layer, wherein the AlGaN covering layer is made of Al 0.4 Ga 0.6 The doping concentration of N and Mg is 1.6x10 19 cm -3 ；
Introducing trimethyl gallium (TMGa) and NH into the reaction cavity under the conditions of reaction pressure of 100mbar and reaction temperature of 950 DEG C 3 And a P-type GaN layer with 150nm thickness is grown by magnesium-cyclopentadienyl (Cp 2 Mg), wherein the doping concentration of Mg is 1 x 10 20 cm -3 ；
And (3) reducing the pressure of the reaction cavity to 30mbar, reducing the temperature to 800 ℃, annealing for 30min under the nitrogen atmosphere, and cooling to room temperature along with the furnace to obtain the ultraviolet LED epitaxial structure.
Example 2
An ultraviolet LED epitaxial structure was prepared in the manner of example 1, except that the reflective metal was silver.
Comparative example 1
An ultraviolet LED epitaxial structure was prepared in the same manner as in example 1 except that the light extraction layer was not included, i.e., a P-type GaN layer having a thickness of 150nm was directly grown on the surface of the hole injection layer.
Performance testing
The ultraviolet LED epitaxial structures obtained in examples 1-2 and comparative example 1 were tested under a drive current of 20mA, and the obtained test results are shown in Table 1;
table 1 test results of uv LED epitaxial structures obtained in examples 1 to 2 and comparative example 1
As can be seen from Table 1, the dislocation in the P-type epitaxial layer is greatly inhibited by growing the light extraction layer, the crystal quality of the P-type epitaxial layer is improved, and meanwhile, the absorption of P-type GaN to light can be greatly reduced, and the light-emitting efficiency of the LED is effectively improved.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (10)
1. The light extraction layer is characterized by comprising an undoped AlGaN layer and a P-type AlGaN covering layer which are sequentially stacked from bottom to top;
the undoped AlGaN layer is provided with a hexagonal defect pit filled with reflective metal; the upper surface of the hexagonal defect pit filled with the reflective metal is in contact with the P-type AlGaN cladding layer.
2. The light extraction layer of claim 1, wherein the undoped AlGaN layer has a thickness of 10 to 20nm;
the thickness of the P-type AlGaN coating layer is 30-50 nm.
3. The light extraction layer of claim 1, wherein the reflective metal comprises one or more of Ag, al, pt, fe and Pd.
4. A method for producing a light extraction layer according to any one of claims 1 to 3, comprising the steps of:
growing an undoped AlGaN layer on the surface of the substrate;
etching the surface of the undoped AlGaN layer to obtain a hexagonal defect pit;
and after depositing reflective metal in the hexagonal defect pits, growing a P-type AlGaN covering layer on the surface of the undoped AlGaN layer to obtain the light extraction layer.
5. The method of claim 4, wherein the undoped AlGaN layer and the P-AlGaN cladding layer are grown by organometallic chemical vapor deposition;
the growth conditions of the undoped AlGaN layer include: the reaction pressure is 20-30 mabr, and the reaction temperature is 1100-1150 ℃;
the growth conditions of the P-type AlGaN coating layer comprise: the reaction pressure is 20-30 mabr, and the reaction temperature is 1100-1150 ℃.
6. The method according to claim 4, wherein the etchant used for the etching comprises an aqueous KOH solution or an aqueous NaOH solution;
the conditions for depositing the reflective metal include: working pressure of 1.0X10 -6 ~4.0×10 -6 The Torr, the output power of the electron gun is 3-4 kW, and the coating power is 0.3-0.4 times of the output power of the electron gun.
7. Use of the light extraction layer according to any one of claims 1 to 3 or the light extraction layer prepared by the preparation method according to any one of claims 4 to 6 in an ultraviolet LED epitaxial structure.
8. The ultraviolet LED epitaxial structure is characterized by comprising a substrate, an AlN buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a multiple quantum well layer, an electron blocking layer, a hole injection layer, a light extraction layer and a P-type GaN layer which are sequentially stacked;
the light extraction layer is the light extraction layer of any one of claims 1-3 or the light extraction layer prepared by the preparation method of any one of claims 4-6;
and the undoped AlGaN layer in the light extraction layer is contacted with the hole injection layer, and the P-type AlGaN covering layer is contacted with the P-type GaN layer.
9. The ultraviolet LED epitaxial structure of claim 8, wherein the AlN buffer layer has a thickness of 4-6 μm;
the thickness of the undoped AlGaN layer is 2-3 mu m;
the thickness of the N-type AlGaN layer is 1-2 mu m;
the multi-quantum well layer comprises a quantum well light-emitting layer and a quantum barrier layer which are alternately stacked; the number of periods of the alternate lamination is 5; in a single period, the thickness of the quantum well light-emitting layer is 2.5nm, and the thickness of the quantum barrier layer is 13nm;
the thickness of the electron blocking layer is 30-50 nm;
the thickness of the hole injection layer is 20-30 nm;
the thickness of the P-type GaN layer is 150-300 nm.
10. The method for preparing the ultraviolet LED epitaxial structure according to claim 8 or 9, comprising the steps of:
and sequentially growing an AlN buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a multi-quantum well layer, an electron blocking layer, a hole injection layer, a light extraction layer and a P-type GaN layer on the surface of the substrate, and annealing to obtain the ultraviolet LED epitaxial structure.
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