CN116072784B - Deep ultraviolet light-emitting diode epitaxial wafer, preparation method thereof and LED - Google Patents

Deep ultraviolet light-emitting diode epitaxial wafer, preparation method thereof and LED Download PDF

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CN116072784B
CN116072784B CN202310319632.3A CN202310319632A CN116072784B CN 116072784 B CN116072784 B CN 116072784B CN 202310319632 A CN202310319632 A CN 202310319632A CN 116072784 B CN116072784 B CN 116072784B
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dimensional
emitting diode
ultraviolet light
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CN116072784A (en
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张彩霞
印从飞
程金连
刘春杨
胡加辉
金从龙
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Jiangxi Zhao Chi Semiconductor Co Ltd
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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
    • H01L33/14—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 carrier transport control structure, e.g. highly-doped semiconductor layer or current-blocking structure
    • 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
    • H01L33/0066—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
    • 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
    • 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
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses a deep ultraviolet light-emitting diode epitaxial wafer and a preparation method thereof, and an LED, wherein the deep ultraviolet light-emitting diode epitaxial wafer comprises a substrate, and a buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a first insertion layer, a multiple quantum well layer, a second insertion layer, an electron blocking layer, a P-type AlGaN layer and an ohmic contact layer which are sequentially laminated on the substrate; the first insertion layer comprises a first MgN three-dimensional layer, an N-type three-dimensional merging layer and an N-type defect healing layer which are sequentially stacked on the N-type AlGaN layer, and the second insertion layer comprises a second MgN three-dimensional layer, a P-type three-dimensional merging layer and a P-type defect healing layer which are sequentially stacked on the multiple quantum well layer. The deep ultraviolet light-emitting diode epitaxial wafer provided by the invention can increase the light-emitting efficiency of the deep ultraviolet light-emitting diode.

Description

Deep ultraviolet light-emitting diode epitaxial wafer, preparation method thereof and LED
Technical Field
The invention relates to the technical field of photoelectricity, in particular to a deep ultraviolet light-emitting diode epitaxial wafer, a preparation method thereof and an LED.
Background
Ultraviolet light emitting diodes (UVLEDs) have wide market application prospects in the fields of biomedical science, anti-counterfeiting identification, purification (water, air and the like), computer data storage, military and the like.
The energy levels of the donor and acceptor impurities in the AlGaN material are deeper than those of GaN, and as the Al component is increased, the forbidden bandwidth of the AlGaN material is increased, the energy level of the donor/acceptor is continuously increased, the activation energy is continuously increased, the carrier activation efficiency and concentration are reduced, and the further application of the deep ultraviolet light-emitting diode is restricted due to low light-emitting efficiency.
Disclosure of Invention
The invention aims to solve the technical problem of providing a deep ultraviolet light-emitting diode epitaxial wafer which can increase the light-emitting efficiency of a deep ultraviolet LED.
The invention also aims to provide a preparation method of the deep ultraviolet light-emitting diode epitaxial wafer, which has simple process and can stably prepare the deep ultraviolet light-emitting diode epitaxial wafer with good luminous efficiency.
In order to solve the technical problems, the invention provides a deep ultraviolet light emitting diode epitaxial wafer, which comprises a substrate, and a buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a first insertion layer, a multiple quantum well layer, a second insertion layer, an electron blocking layer, a P-type AlGaN layer and an ohmic contact layer which are sequentially laminated on the substrate;
the first insertion layer comprises a first MgN three-dimensional layer, an N-type three-dimensional merging layer and an N-type defect healing layer which are sequentially laminated on the N-type AlGaN layer, wherein the N-type three-dimensional merging layer comprises alternately laminated Al x Ga 1-x An N layer and an N-type GaN layer, the N-type defect healing layer comprising a first InN layer and an N-type Al layer alternately laminated y Ga 1-y An N layer, wherein the value range of x is 0.1-0.6, and the value range of y is 0.1-0.6;
the second insertion layer comprises a second MgN three-dimensional layer, a P-type three-dimensional merging layer and a P-type defect healing layer which are sequentially laminated on the multiple quantum well layer, wherein the P-type three-dimensional merging layer comprises alternately laminated Al a Ga 1-a An N layer and a P-type GaN layer, wherein the P-type defect healing layer comprises a second InN layer and a P-type Al layer which are alternately laminated b Ga 1-b And an N layer, wherein the value range of a is 0.1-0.6, and the value range of b is 0.1-0.6.
In one embodiment, the thickness of the first MgN three-dimensional layer is 3 nm-10 nm;
the thickness of the second MgN three-dimensional layer is 3 nm-10 nm.
In one embodiment, the Al x Ga 1-x Alternating of N layers and N-type GaN layersThe laminated cycle number is 5-20;
the Al is x Ga 1-x The thickness of the N layer is 1 nm-10 nm;
the thickness of the N-type GaN layer is 1 nm-10 nm;
the doping concentration of the N-type GaN layer is 1 multiplied by 10 16 atoms/cm 3 ~1×10 17 atoms/cm 3 。
In one embodiment, the first InN layer and the N-type Al y Ga 1-y The number of periods of the alternate lamination of the N layers is 1-6;
the thickness of the first InN layer is 0.1 nm-3 nm;
the N type Al y Ga 1-y The thickness of the N layer is 10 nm-20 nm;
the N type Al y Ga 1-y The doping concentration of the N layer is 1 multiplied by 10 15 atoms/cm 3 ~1×10 16 atoms/cm 3 。
In one embodiment, the Al a Ga 1-a The periodicity of the alternate lamination of the N layer and the P-type GaN layer is 5-20;
the Al is a Ga 1-a The thickness of the N layer is 1 nm-5 nm;
the thickness of the P-type GaN layer is 1 nm-5 nm;
the doping concentration of the P-type GaN layer is 1 multiplied by 10 17 atoms/cm 3 ~1×10 18 atoms/cm 3 。
In one embodiment, the second InN layer and the P-type Al b Ga 1-b The number of periods of the alternate lamination of the N layers is 1-6;
the thickness of the second InN layer is 0.1 nm-3 nm;
the P type Al b Ga 1-b The thickness of the N layer is 10 nm-20 nm;
the P type Al b Ga 1-b The doping concentration of the N layer is 1 multiplied by 10 16 atoms/cm 3 ~1×10 17 atoms/cm 3 。
In order to solve the problems, the invention provides a preparation method of a deep ultraviolet light emitting diode epitaxial wafer, which comprises the following steps:
s1, preparing a substrate;
s2, sequentially depositing a buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a first insertion layer, a multiple quantum well layer, a second insertion layer, an electron blocking layer, a P-type AlGaN layer and an ohmic contact layer on the substrate;
depositing a first insertion layer on the N-type AlGaN layer, comprising the following steps:
sequentially depositing a first MgN three-dimensional layer, an N three-dimensional merging layer and an N-type defect healing layer on the N-type AlGaN layer, wherein the N three-dimensional merging layer comprises alternately laminated Al x Ga 1-x An N layer and an N-type GaN layer, the N-type defect healing layer comprising a first InN layer and an N-type Al layer alternately laminated y Ga 1-y An N layer, wherein the value range of x is 0.1-0.6, and the value range of y is 0.1-0.6;
depositing a second insertion layer on the multiple quantum well layer, comprising the steps of:
sequentially depositing a second MgN three-dimensional layer, a P-type three-dimensional merging layer and a P-type defect healing layer on the multiple quantum well layer, wherein the P-type three-dimensional merging layer comprises alternately laminated Al a Ga 1-a An N layer and a P-type GaN layer, wherein the P-type defect healing layer comprises a second InN layer and a P-type Al layer which are alternately laminated b Ga 1-b And an N layer, wherein the value range of a is 0.1-0.6, and the value range of b is 0.1-0.6.
In one embodiment, sequentially depositing a first MgN three-dimensional layer on the N-type AlGaN layer or sequentially depositing a second MgN three-dimensional layer on the multiple quantum well layer, comprises the steps of:
controlling the temperature of the reaction chamber to be 700-800 ℃, and introducing N 2 And (3) introducing a Mg source and an N source as carrier gas, wherein the Mg source is introduced in a pulse manner, so as to finish deposition.
In one embodiment, the growth temperature of the N-type three-dimensional merging layer is 1030-1070 ℃;
the growth temperature of the P-type three-dimensional merging layer is 1030-1070 ℃;
the growth temperature of the first InN layer is 900-1000 ℃;
the N type Al y Ga 1-y The temperature of the N layer is 1100-1200 ℃;
the growth temperature of the second InN layer is 1000-1050 ℃;
the P type Al b Ga 1-b The growth temperature of the N layer is 1100-1200 ℃.
Correspondingly, the invention also provides an LED, and the LED comprises the deep ultraviolet light emitting diode epitaxial wafer.
The implementation of the invention has the following beneficial effects:
the invention provides a deep ultraviolet light-emitting diode epitaxial wafer, which is provided with a first insertion layer and a second insertion layer respectively arranged at the front and the back of a multiple quantum well layer, wherein the first insertion layer comprises a first MgN three-dimensional layer, an N-type three-dimensional merging layer and an N-type defect healing layer which are sequentially laminated on an N-type AlGaN layer, and the N-type three-dimensional merging layer comprises alternately laminated Al x Ga 1-x An N layer and an N-type GaN layer, the N-type defect healing layer comprising a first InN layer and an N-type Al layer alternately laminated y Ga 1-y And N layers. The second insertion layer comprises a second MgN three-dimensional layer, a P-type three-dimensional merging layer and a P-type defect healing layer which are sequentially laminated on the multiple quantum well layer, wherein the P-type three-dimensional merging layer comprises alternately laminated Al a Ga 1-a An N layer and a P-type GaN layer, wherein the P-type defect healing layer comprises a second InN layer and a P-type Al layer which are alternately laminated b Ga 1-b And N layers.
The first MgN three-dimensional layer and the second MgN three-dimensional layer can cause surface roughening, so that total reflection severity of light rays is reduced, diffuse reflection at an MgN roughened interface is increased, and light extraction efficiency is increased. The first insertion layer and the second insertion layer can increase the concentration of holes, the mobility of the holes and the expansion of the holes entering the multi-quantum well region, increase the expansion of electrons entering the multi-quantum well region, balance the concentration of the electrons and the holes of the multi-quantum well region, and therefore increase the luminous efficiency of the deep ultraviolet light emitting diode.
Drawings
Fig. 1 is a schematic structural diagram of a deep ultraviolet light emitting diode epitaxial wafer provided by the invention;
fig. 2 is a schematic structural diagram of a first interposer of the deep ultraviolet led epitaxial wafer provided by the present invention;
fig. 3 is a schematic structural diagram of a second interposer of the deep ultraviolet led epitaxial wafer provided by the present invention;
fig. 4 is a flowchart of a preparation method of a deep ultraviolet light emitting diode epitaxial wafer provided by the invention;
fig. 5 is a flowchart of step S2 of the preparation method of the deep ultraviolet light emitting diode epitaxial wafer provided by the invention.
Wherein: the substrate 1, the buffer layer 2, the undoped AlGaN layer 3, the N-type AlGaN layer 4, the first insertion layer 5, the multiple quantum well layer 6, the second insertion layer 7, the electron blocking layer 8, the P-type AlGaN layer 9, the ohmic contact layer 10, the first MgN three-dimensional layer 51, the N-type three-dimensional merging layer 52 and the N-type defect healing layer 53, the second MgN three-dimensional layer 71, the P-type three-dimensional merging layer 72 and the P-type defect healing layer 73.
Detailed Description
The present invention will be described in further detail below in order to make the objects, technical solutions and advantages of the present invention more apparent.
Unless otherwise indicated or contradicted, terms or phrases used herein have the following meanings:
in the present invention, "preferred" is merely to describe embodiments or examples that are more effective, and it should be understood that they are not intended to limit the scope of the present invention.
In the invention, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.
In the present invention, the numerical range is referred to, and both ends of the numerical range are included unless otherwise specified.
As the forbidden bandwidth of the AlGaN material is increased, the energy level of a donor/acceptor is deepened continuously, the activation energy is increased continuously, the carrier activation efficiency and concentration are reduced, and the efficiency of the deep ultraviolet light-emitting diode with the traditional epitaxial structure is lower at the present stage.
In order to solve the above problems, the present invention provides a deep ultraviolet light emitting diode epitaxial wafer, as shown in fig. 1-3, comprising a substrate 1, and a buffer layer 2, an undoped AlGaN layer 3, an N-type AlGaN layer 4, a first insertion layer 5, a multiple quantum well layer 6, a second insertion layer 7, an electron blocking layer 8, a P-type AlGaN layer 9 and an ohmic contact layer 10 which are sequentially stacked on the substrate 1;
the first insertion layer 5 comprises a first MgN three-dimensional layer 51, an N-type three-dimensional merging layer 52 and an N-type defect healing layer 53 which are sequentially laminated on the N-type AlGaN layer 4, wherein the N-type three-dimensional merging layer 52 comprises alternately laminated Al x Ga 1-x An N layer and an N-type GaN layer, the N-type defect healing layer 53 comprising a first InN layer and an N-type Al layer alternately laminated y Ga 1-y An N layer, wherein the value range of x is 0.1-0.6, and the value range of y is 0.1-0.6; exemplary values of x are, but not limited to, 0.2, 0.3, 0.4, 0.5. Exemplary values of y are, but not limited to, 0.2, 0.3, 0.4, 0.5.
The second insertion layer 7 includes a second MgN three-dimensional layer 71, a P-type three-dimensional merging layer 72 and a P-type defect healing layer 73 sequentially laminated on the multiple quantum well layer 6, the P-type three-dimensional merging layer 72 including alternately laminated Al a Ga 1-a An N layer and a P-type GaN layer, the P-type defect healing layer 73 comprising a second InN layer and a P-type Al layer alternately laminated b Ga 1-b And an N layer, wherein the value range of a is 0.1-0.6, and the value range of b is 0.1-0.6. Exemplary values of a are, but not limited to, 0.2, 0.3, 0.4, 0.5. Exemplary values of b are, but not limited to, 0.2, 0.3, 0.4, 0.5.
In one embodiment, the thickness of the first MgN three-dimensional layer 51 is 3nm to 10nm; the thickness of the second MgN three-dimensional layer 71 is 3nm to 10nm. Exemplary thicknesses of the first MgN three-dimensional layer 51 are 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, but are not limited thereto. Exemplary thicknesses of the second MgN three-dimensional layer 71 are 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, but are not limited thereto. The roughened surfaces caused by the first MgN three-dimensional layer 51 and the second MgN three-dimensional layer 71 reduce total reflection severity of light rays, and increase diffuse reflection at MgN roughened interfaces. Light extraction efficiency since a large amount of light emitted from the quantum well is confined inside the LED and absorbed by the epitaxial material due to the high refractive index of the nitride material, resulting in very low light extraction efficiency, the first MgN three-dimensional layer 51 and the second MgN three-dimensional layer 71 provided at both ends of the multiple quantum well layer 6 correspond to mirrors provided at both ends of the multiple quantum well layer 6, and thus the light extraction efficiency is greatly increased.
As shown in fig. 2, the first interposer layer 5 further includes an N-type three-dimensional consolidated layer 52 and an N-type defect healing layer 53 in addition to the first MgN three-dimensional layer 51, and specific structures of the N-type three-dimensional consolidated layer 52 and the N-type defect healing layer 53 are as follows:
in one embodiment, the Al of the N-type three-dimensional consolidated layer 52 x Ga 1-x The periodicity of the alternate lamination of the N layer and the N-type GaN layer is 5-20; exemplary cycle numbers are 8, 10, 12, 15, 18, 19, but are not limited thereto. In one embodiment, the Al x Ga 1-x The thickness of the N layer is 1 nm-10 nm, and the Al is exemplified x Ga 1-x The thickness of the N layer is 2nm, 3nm, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, but not limited thereto. In one embodiment, the thickness of the N-type GaN layer is 1nm to 10nm, and exemplary N-type GaN layers are 2nm, 3nm, 4nm, 5nm, 6nm, 7nm, 8nm, 9nm, but not limited thereto. In one embodiment, the doping concentration of the N-type GaN layer is 1×10 16 atoms/cm 3 ~1×10 17 atoms/cm 3 Exemplary doping concentrations of the N-type GaN layer are 2×10 16 atoms/cm 3 、4×10 16 atoms/cm 3 、6×10 16 atoms/cm 3 、8×10 16 atoms/cm 3 But is not limited thereto.
In one embodiment, the first InN layer of the N-type defect healing layer 53 and N-type Al y Ga 1-y The number of periods of the alternating lamination of the N layers is 1-6, and the exemplary number of periods is 2, 3, 4 and 5, but is not limited thereto; the thickness of the first InN layer is 0.1 nm-3 nm, and exemplary thicknesses of the first InN layer are 0.2nm, 0.5nm, 0.8nm, 1nm, 1.5nm, 2nm, 2.5nm, but are not limited thereto; the N type Al y Ga 1-y The thickness of the N layer is 10 nm-20 nm, and the N type Al is exemplified y Ga 1-y The N layer is 12nm, 14nm, 16nm, 18nmBut is not limited thereto; the N type Al y Ga 1-y The doping concentration of the N layer is 1 multiplied by 10 15 atoms/cm 3 ~1×10 16 atoms/cm 3 Exemplary of the N-type Al y Ga 1-y The doping concentration of the N layer is 2 multiplied by 10 15 atoms/cm 3 、4×10 15 atoms/cm 3 、6×10 15 atoms/cm 3 、8×10 15 atoms/cm 3 But is not limited thereto.
The first insertion layer 5 is provided to increase the electron expansion into the multiple quantum well layer 6 and balance the electron and hole concentrations of the multiple quantum well layer 6. When electrons generated by the N-type AlGaN layer 4 pass through the three-dimensional layer in the first insertion layer 5, the three-dimensional structure increases the electron expansion area, which is beneficial to increasing the electron expansion; the N-type three-dimensional combined layer 52 is matched with the N-type GaN layer doped with low Si by virtue of the specific laminated structure, thereby being beneficial to increasing conductivity and increasing the effect of electron expansion. In the N-type defect healing layer 53, the first InN layer can reduce the surface energy of the material, increase the mobility of Al atoms, repair defects generated during three-dimensional filling and leveling, and improve the lattice quality. And the InN energy level is lower, so that the InN energy level can become an electron trap, the electron moving speed is slowed down, the electron overflow is prevented, and the electron can be better expanded. In summary, the first insertion layer 5 is configured to increase the electron expansion into the multiple quantum well layer 6, and balance the electron and hole concentrations of the multiple quantum well layer 6.
Further, as shown in fig. 3, the second interposer 7 includes a P-type three-dimensional merging layer 72 and a P-type defect healing layer 73 in addition to the second MgN three-dimensional layer 71, and specific structures of the P-type three-dimensional merging layer 72 and the P-type defect healing layer 73 are as follows:
in one embodiment, the Al of the P-type three-dimensional consolidated layer 72 a Ga 1-a The periodicity of the alternate lamination of the N layer and the P-type GaN layer is 5-20; exemplary cycle numbers are 8, 10, 12, 15, 18, 19, but are not limited thereto. In one embodiment, the Al a Ga 1-a The thickness of the N layer is 1 nm-5 nm, and the Al is exemplified a Ga 1-a The thickness of the N layer is 2nm, 3nm, 4nm, but not limited thereto. In one embodiment, the thickness of the P-type GaN layer is 1nm to 5nm, and exemplary thicknesses of the P-type GaN layer are 2nm, 3nm, and 4nm, but not limited thereto. In one embodiment, the doping concentration of the P-type GaN layer is 1×10 17 atoms/cm 3 ~1×10 18 atoms/cm 3 Exemplary doping concentrations of the P-type GaN layer are 2×10 17 atoms/cm 3 、4×10 17 atoms/cm 3 、6×10 17 atoms/cm 3 、8×10 17 atoms/cm 3 But is not limited thereto.
In one embodiment, the second InN layer of the P-type defect healing layer 73 and P-type Al b Ga 1-b The number of periods of the alternating lamination of the N layers is 1-6, and the exemplary number of periods is 2, 3, 4 and 5, but is not limited thereto; the thickness of the second InN layer is 0.1 nm-3 nm, and exemplary thicknesses of the second InN layer are 0.2nm, 0.5nm, 0.8nm, 1nm, 1.5nm, 2nm, 2.5nm, but are not limited thereto; the P type Al b Ga 1-b The thickness of the N layer is 10 nm-20 nm, and the P type Al is exemplified b Ga 1-b The N layer is 12nm, 14nm, 16nm and 18nm, but is not limited thereto; the P type Al b Ga 1-b N has a doping concentration of 1×10 16 atoms/cm 3 ~1×10 17 atoms/cm 3 Exemplary of the P-type Al b Ga 1-b N has a doping concentration of 2×10 16 atoms/cm 3 、4×10 16 atoms/cm 3 、6×10 16 atoms/cm 3 、8×10 16 atoms/cm 3 But is not limited thereto.
The second insertion layer 7 can increase the concentration of holes entering the multiple quantum well region, the mobility of holes, and the expansion of holes. The acceptor impurity energy level in the deep ultraviolet AlGaN material is deeper than that of GaN, and as the Al component is increased, the forbidden bandwidth of the AlGaN material is increased, the acceptor energy level is continuously deepened, the activation energy can be continuously increased, and the carrier activation efficiency and concentration are reduced. The second insertion layer 7 of the present invention adopts superlattice materials as a three-dimensional merging layer and a three-dimensional healing layer, a polarized electric field is formed in the heterogeneous superlattice materials, and energy band bending induced by the polarized electric field can reduce donor energy level and increase activation rate of Mg atoms, thereby increasing hole concentration. And the three-dimensional merging layer and the three-dimensional healing layer formed by the heterogeneous superlattice material of the second insertion layer 7 can form two-dimensional hole gas, so that the hole mobility is greatly improved. The three-dimensional consolidated layer is referred to herein as the P-type three-dimensional consolidated layer 72, and the three-dimensional consolidated layer is referred to herein as the P-type defect consolidated layer 73. Further, in the P-type defect healing layer 73, the P-type doped AlGaN may generate holes, but the activation rate of Mg is low, and the hole expansion is poor due to the viscous effect of Al atoms, in atoms In the InN material may increase the activation rate of Mg atoms, so that the hole concentration is greatly increased, and InN has poor stability, so that the surface energy of the material can be reduced, the mobility of Al atoms is increased, the defects generated during three-dimensional filling and leveling are repaired, the lattice quality is improved, the consumption of carriers by the defects is reduced, and the light emitting efficiency is improved. Mg atoms are contained in each sub-layer of the second insertion layer 7, increasing the concentration of holes into the multiple quantum well region.
In summary, the first interposer layer 5 and the second interposer layer 7 are added before and after the multiple quantum well layer 6, where the first MgN three-dimensional layer 51 and the second MgN three-dimensional layer 71 can cause surface roughening, so as to reduce total reflection severity of light, increase diffuse reflection at MgN roughened interfaces, and increase light extraction efficiency. The first insertion layer 5 and the second insertion layer 7 can increase the concentration of holes, the mobility of holes and the expansion of holes entering the multi-quantum well region, increase the expansion of electrons entering the multi-quantum well region, balance the concentration of electrons and holes in the multi-quantum well region, and thus increase the luminous efficiency of the deep ultraviolet light emitting diode.
Correspondingly, the invention provides a preparation method of a deep ultraviolet light-emitting diode epitaxial wafer, which is shown in fig. 4 and comprises the following steps:
s1, preparing a substrate 1;
in one embodiment, the substrate is a sapphire substrate. Sapphire is the most commonly used substrate material at present, and the sapphire substrate has the advantages of mature preparation process, low price, easy cleaning and processing and good stability at high temperature.
S2, a buffer layer 2, an undoped AlGaN layer 3, an N-type AlGaN layer 4, a first insertion layer 5, a multiple quantum well layer 6, a second insertion layer 7, an electron blocking layer 8, a P-type AlGaN layer 9 and an ohmic contact layer 10 are sequentially deposited on the substrate 1.
As shown in fig. 5, step S2 includes the steps of:
s21, growing a buffer layer 2 on the substrate 1, including:
in one embodiment, an AlN material is employed as the buffer layer. Preferably, the AlN buffer layer may be obtained by a magnetron sputtering method. The AlN buffer layer with better quality can be obtained by controlling the sputtering temperature of PVD equipment to be 400-700 ℃, the power to be 3000-5000W and the pressure to be 1-10 torr.
S22, depositing an undoped AlGaN layer 3 on the buffer layer 2.
In one embodiment, transferring the epitaxial wafer plated with the AlN buffer layer into MOCVD equipment, controlling the growth temperature of a reaction cavity to be 1000-1200 ℃ and the growth pressure to be 100-500 torr and H 2 And N 2 Introducing NH under the condition that the mixed gas is used as carrier gas 3 The growth thickness of the Al source and the Ga source is 1-5 mu m. Preferably, the growth temperature is 1100 ℃, the growth pressure is 200torr, and the growth thickness is 3 μm. The undoped AlGaN layer has higher growth temperature and lower pressure, and the prepared crystal has better quality.
S23, depositing an N-type AlGaN layer 4 on the undoped AlGaN layer 3.
In one embodiment, the growth temperature of the reaction chamber is controlled to be 1000-1350 ℃, the growth pressure is 100-500 torr, the N type is doped into Si, and the doping concentration of Si is 1X 10 19 atoms/cm 3 ~5×10 19 atoms/cm 3 。H 2 And N 2 The mixed gas is used as carrier gas, and SiH is simultaneously introduced into the reaction chamber 4 The growth thickness of the source, ga source, al source and ammonia gas is 1-5 mu m.
Preferably, the growth temperature is 1250 ℃, the growth pressure is 150torr, the growth thickness is 3 μm, and the Si doping concentration is 2.6X10 19 atoms/cm 3 Thus, itCan provide enough electrons for the ultraviolet LED to emit light.
And S24, depositing a first insertion layer 5 on the N-type AlGaN layer 4.
In one embodiment, the method comprises the steps of:
controlling the temperature of the reaction chamber to be 700-800 ℃, and introducing N 2 As carrier gas, introducing a Mg source and an N source, wherein the Mg source is introduced in a pulse manner, so as to complete the deposition of the first MgN three-dimensional layer 51;
then controlling the growth temperature of the reaction chamber to 1030-1070 ℃ and the growth pressure to 200-500 torr, and introducing H 2 And N 2 The mixed gas is used as carrier gas, and is introduced with an N source, an Al source and a Ga source to grow the Al x Ga 1-x And closing an Al source, continuously introducing the N source, the Ga source and the doping source, growing the N-type GaN layer, and alternately stacking the Al x Ga 1-x An N layer and an N-type GaN layer to obtain the N-type three-dimensional merged layer 52;
then, the temperature of the reaction chamber is controlled to be 900-1000 ℃ and the growth pressure is controlled to be 50-200 torr, and H is introduced 2 And N 2 The mixed gas is used as carrier gas, an N source and an In source are introduced, and the first InN layer is grown; then closing an In source, controlling the temperature of a reaction chamber to be 1100-1200 ℃, introducing an N source, an Al source, a Ga source and a doping source, and growing the N-type Al y Ga 1-y An N layer; alternately stacking the first InN layer and the N-type Al layer y Ga 1-y An N layer, obtaining the N-type defect healing layer 53;
the growth temperature of the first InN layer is too high, so that In atoms are quickly desorbed; the N type Al y Ga 1-y The higher growth temperature of the N layer is beneficial to improving the quality of the crystal lattice. The low pressure is beneficial to two-dimensional growth, and the lattice quality is higher.
S25, depositing a multiple quantum well layer 6 on the first insertion layer 5.
The multiple quantum well layer 6 is an active region of the deep ultraviolet light emitting diode, and is a region where electrons and holes are recombined, and has a great influence on the light emitting efficiency of the light emitting diode. In one embodiment, the multiple quantum well layers are alternately stacked Al m Ga 1- m N quantum well layer and Al n Ga 1-n N quantum barrier layers, stacking 6-12 periods; h 2 And N 2 And (3) taking the mixed gas as carrier gas, introducing a Ga source, an Al source and ammonia gas into the reaction chamber, controlling the growth pressure to be 50-300 torr, and controlling the growth temperature to be 900-1200 ℃ to grow the multi-quantum well layer. Wherein the Al is m Ga 1-m The thickness of the N quantum well layer is 2 nm-5 nm, and the value range of m is 0.2-0.6; the Al is n Ga 1-n The thickness of the N quantum barrier layer is 5 nm-15 nm, and the value range of N is 0.4-0.8.
Preferably, the stacking cycle number is 9, the Al m Ga 1-m The thickness of the N quantum well layer is 3nm, the Al n Ga 1-n The thickness of the N quantum barrier layer is 10nm, the growth pressure is 200torr, and the growth temperature is 1100 ℃.
S26, depositing a second insertion layer 7 on the multiple quantum well layer 6.
In one embodiment, the method comprises the steps of:
controlling the temperature of the reaction chamber to be 700-800 ℃, and introducing N 2 As carrier gas, introducing a Mg source and an N source, wherein the Mg source is introduced in a pulse manner, so as to complete the deposition of the second MgN three-dimensional layer 71;
then controlling the growth temperature of the reaction chamber to 1030-1070 ℃ and the growth pressure to 200-500 torr, and introducing H 2 And N 2 The mixed gas is used as carrier gas, and is introduced with an N source, an Al source and a Ga source to grow the Al a Ga 1-a N layer, closing Al source, continuously introducing N source, ga source and doping source, growing P-type GaN layer, alternately laminating Al a Ga 1-a An N layer and a P-type GaN layer to obtain the P-type three-dimensional merged layer 72;
then, firstly controlling the temperature of the reaction chamber to be 1000-1050 ℃ and the growth pressure to be 50-200 torr, and introducing H 2 And N 2 The mixed gas is used as carrier gas, an N source and an In source are introduced, and the second InN layer is grown; then closing an In source, controlling the temperature of a reaction chamber to be 1100-1200 ℃, and introducing an N source, an Al source, a Ga source and a doping source to grow the P-type Al b Ga 1-b An N layer; alternately stacking the second InN layer and the P-type Al layer b Ga 1-b An N layer for obtaining the P-type defect healing layer73。
The growth temperature of the second InN layer is too high, so that In atoms are quickly desorbed; the P type Al b Ga 1-b The higher growth temperature of the N layer is beneficial to improving the quality of the crystal lattice. The low pressure is beneficial to two-dimensional growth, and the lattice quality is higher.
And S27, depositing an electron blocking layer 8 on the second insertion layer 7.
In one embodiment, the electron blocking layer is an AlGaN electron blocking layer, the thickness is 10 nm-100 nm, the growth temperature is 1000-1200 ℃, the pressure is 150-300 torr, and the Al component is 0.4-0.7.
Preferably, the thickness of the AlGaN electron blocking layer is 40nm, wherein the Al component is 0.6, the growth temperature is 1050 ℃, and the growth pressure is 200torr, so that the prepared AlGaN electron blocking layer can not only effectively limit electron overflow, but also reduce blocking of holes, improve injection efficiency of holes to quantum wells, reduce carrier auger recombination, and improve luminous efficiency of the light-emitting diode.
And S28, depositing a P-type AlGaN layer 9 on the electron blocking layer 8.
In one embodiment, the growth temperature of the reaction chamber is controlled to be 1000-1200 ℃, and the growth pressure is controlled to be 100-600 torr, H 2 And N 2 The mixed gas is used as carrier gas, ga source, al source and N source are introduced, a P-type AlGaN layer is grown, the thickness of the P-type AlGaN layer is 10 nm-100 nm, and the doping concentration of P-type doped Mg is 1 multiplied by 10 19 atoms/cm 3 ~1×10 20 atoms/cm 3 。
Preferably, the growth temperature of the P-type AlGaN layer is 1100 ℃, the thickness is 50nm, the growth pressure is 200torr, and the doping concentration of Mg is 5 multiplied by 10 19 atoms/cm 3 The layer mainly provides holes for the deep ultraviolet light emitting diode.
And S29, depositing an ohmic contact layer 10 on the P-type AlGaN layer 9.
In one embodiment, the growth temperature of the reaction chamber is controlled to be 1000-1100 ℃, the growth pressure is 100-600 torr, and H 2 And N 2 The mixed gas is used as carrier gas, ga source, al source and N source are introduced into the reaction chamber, the growth thickness is 10nm-50nm, and the doping concentration of P-doped Mg is5×10 19 atoms/cm 3 -5×10 20 atoms/cm 3 。
Preferably, the growth temperature is 1050 ℃, the thickness is 20nm, the growth pressure is 200torr, and the doping concentration of Mg is 1 multiplied by 10 20 atoms/cm 3 The P-type contact layer with high doping concentration can reduce contact resistance.
In summary, the preparation method of the deep ultraviolet light-emitting diode epitaxial wafer provided by the invention has a simple process, and the deep ultraviolet light-emitting diode epitaxial wafer with good luminous efficiency can be stably prepared by adopting a specific process. Correspondingly, the invention also provides an LED, which comprises the deep ultraviolet light emitting diode epitaxial wafer. The photoelectric efficiency of the LED is effectively improved, and other items have good electrical properties.
The invention is further illustrated by the following examples:
example 1
The embodiment provides a deep ultraviolet light-emitting diode epitaxial wafer, which comprises a substrate, and a buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a first insertion layer, a multiple quantum well layer, a second insertion layer, an electron blocking layer, a P-type AlGaN layer and an ohmic contact layer which are sequentially laminated on the substrate;
the first insertion layer comprises a first MgN three-dimensional layer, an N-type three-dimensional merging layer and an N-type defect healing layer which are sequentially laminated on the N-type AlGaN layer, wherein the N-type three-dimensional merging layer comprises Al which is alternately laminated for 15 periods x Ga 1-x An N layer and an N-type GaN layer, the N-type defect healing layer comprising a first InN layer and an N-type Al layer alternately laminated for 5 periods y Ga 1-y N layers, wherein x is 0.3 and y is 0.3;
the second insertion layer comprises a second MgN three-dimensional layer, a P-type three-dimensional merging layer and a P-type defect healing layer which are sequentially laminated on the multiple quantum well layer, wherein the P-type three-dimensional merging layer comprises Al which is alternately laminated for 15 periods a Ga 1-a An N layer and a P-type GaN layer, wherein the P-type defect healing layer comprises a second InN layer and a P-type Al layer which are alternately laminated for 5 periods b Ga 1-b N layers, where a is 0.3 and b is 0.3.
Example 2
The present embodiment provides a deep ultraviolet light emitting diode epitaxial wafer, which is different from embodiment 1 in that: a is 0.1, b is 0.1, x is 0.1, and y is 0.1. The remainder was the same as in example 1.
Example 3
The present embodiment provides a deep ultraviolet light emitting diode epitaxial wafer, which is different from embodiment 1 in that a is 0.6, b is 0.6, x is 0.6, and y is 0.6. The remainder was the same as in example 1.
Comparative example 1
This comparative example is different from example 1 in that the first insertion layer is not provided, and the rest is the same as example 1.
Comparative example 2
This comparative example is different from example 1 in that the second insertion layer is not provided, and the rest is the same as example 1.
Comparative example 3
This comparative example is different from example 1 in that the first and second insertion layers are not provided, and the rest is the same as example 1.
The deep ultraviolet light emitting diode epitaxial wafers prepared in examples 1-3 and comparative examples 1-3 were prepared into 10×24mil chips using the same chip process conditions, 300 LED chips were extracted respectively, and the photoelectric properties of the chips were tested, and specific test results are shown in table 1.
TABLE 1 results of Performance test of LEDs made in example 1-example 3 and comparative examples 1-3
Figure SMS_1
From the above results, the deep ultraviolet light emitting diode epitaxial wafer provided by the invention is provided with a first insertion layer and a second insertion layer respectively arranged in front and behind a multiple quantum well layer, wherein the first insertion layer comprises a first MgN three-dimensional layer, an N three-dimensional merging layer and an N defect healing layer which are sequentially laminated on the N-type AlGaN layer, and the N three-dimensional merging layer comprises alternately laminated Al x Ga 1-x An N layer and an N-type GaN layer, wherein the N-type defect healing layer comprises a cross-over layerA first InN layer and N-type Al layer alternately stacked y Ga 1-y And N layers. The second insertion layer comprises a second MgN three-dimensional layer, a P-type three-dimensional merging layer and a P-type defect healing layer which are sequentially laminated on the multiple quantum well layer, wherein the P-type three-dimensional merging layer comprises alternately laminated Al a Ga 1-a An N layer and a P-type GaN layer, wherein the P-type defect healing layer comprises a second InN layer and a P-type Al layer which are alternately laminated b Ga 1-b And N layers.
The first MgN three-dimensional layer and the second MgN three-dimensional layer can cause surface roughening, so that total reflection severity of light rays is reduced, diffuse reflection at an MgN roughened interface is increased, and light extraction efficiency is increased. The first insertion layer and the second insertion layer can increase the concentration of holes, the mobility of the holes and the expansion of the holes entering the multi-quantum well region, increase the expansion of electrons entering the multi-quantum well region, balance the concentration of the electrons and the holes of the multi-quantum well region, and therefore increase the luminous efficiency of the deep ultraviolet light emitting diode.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that changes and modifications may be made without departing from the principles of the invention, such changes and modifications are also intended to be within the scope of the invention.

Claims (10)

1. The deep ultraviolet light-emitting diode epitaxial wafer is characterized by comprising a substrate, and a buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a first insertion layer, a multiple quantum well layer, a second insertion layer, an electron blocking layer, a P-type AlGaN layer and an ohmic contact layer which are sequentially laminated on the substrate;
the first insertion layer comprises a first MgN three-dimensional layer, an N-type three-dimensional merging layer and an N-type defect healing layer which are sequentially laminated on the N-type AlGaN layer, wherein the N-type three-dimensional merging layer comprises alternately laminated Al x Ga 1-x An N layer and an N-type GaN layer, the N-type defect healing layer comprising a first InN layer and an N-type Al layer alternately laminated y Ga 1-y An N layer, wherein the value range of x is 0.1-0.6, and the value range of y is 0.1-0.6;
the second plugThe embedded layer comprises a second MgN three-dimensional layer, a P-type three-dimensional merging layer and a P-type defect healing layer which are sequentially laminated on the multiple quantum well layer, wherein the P-type three-dimensional merging layer comprises alternately laminated Al a Ga 1-a An N layer and a P-type GaN layer, wherein the P-type defect healing layer comprises a second InN layer and a P-type Al layer which are alternately laminated b Ga 1-b And an N layer, wherein the value range of a is 0.1-0.6, and the value range of b is 0.1-0.6.
2. The deep ultraviolet light-emitting diode epitaxial wafer of claim 1, wherein the thickness of the first MgN three-dimensional layer is 3nm to 10nm;
the thickness of the second MgN three-dimensional layer is 3 nm-10 nm.
3. The deep ultraviolet light-emitting diode epitaxial wafer of claim 1, wherein the Al x Ga 1-x The periodicity of the alternate lamination of the N layer and the N-type GaN layer is 5-20;
the Al is x Ga 1-x The thickness of the N layer is 1 nm-10 nm;
the thickness of the N-type GaN layer is 1 nm-10 nm;
the doping concentration of the N-type GaN layer is 1 multiplied by 10 16 atoms/cm 3 ~1×10 17 atoms/cm 3 。
4. The deep ultraviolet light-emitting diode epitaxial wafer of claim 1, wherein the first InN layer and N-type Al y Ga 1-y The number of periods of the alternate lamination of the N layers is 1-6;
the thickness of the first InN layer is 0.1 nm-3 nm;
the N type Al y Ga 1-y The thickness of the N layer is 10 nm-20 nm;
the N type Al y Ga 1-y The doping concentration of the N layer is 1 multiplied by 10 15 atoms/cm 3 ~1×10 16 atoms/cm 3 。
5. The deep ultraviolet light-emitting diode epitaxial wafer of claim 1, wherein the Al a Ga 1-a The periodicity of the alternate lamination of the N layer and the P-type GaN layer is 5-20;
the Al is a Ga 1-a The thickness of the N layer is 1 nm-5 nm;
the thickness of the P-type GaN layer is 1 nm-5 nm;
the doping concentration of the P-type GaN layer is 1 multiplied by 10 17 atoms/cm 3 ~1×10 18 atoms/cm 3 。
6. The deep ultraviolet light-emitting diode epitaxial wafer of claim 1, wherein the second InN layer and P-type Al b Ga 1-b The number of periods of the alternate lamination of the N layers is 1-6;
the thickness of the second InN layer is 0.1 nm-3 nm;
the P type Al b Ga 1-b The thickness of the N layer is 10 nm-20 nm;
the P type Al b Ga 1-b The doping concentration of the N layer is 1 multiplied by 10 16 atoms/cm 3 ~1×10 17 atoms/cm 3 。
7. The preparation method of the deep ultraviolet light-emitting diode epitaxial wafer is characterized by comprising the following steps of:
s1, preparing a substrate;
s2, sequentially depositing a buffer layer, an undoped AlGaN layer, an N-type AlGaN layer, a first insertion layer, a multiple quantum well layer, a second insertion layer, an electron blocking layer, a P-type AlGaN layer and an ohmic contact layer on the substrate;
depositing a first insertion layer on the N-type AlGaN layer, comprising the following steps:
sequentially depositing a first MgN three-dimensional layer, an N three-dimensional merging layer and an N-type defect healing layer on the N-type AlGaN layer, wherein the N three-dimensional merging layer comprises alternately laminated Al x Ga 1-x An N layer and an N-type GaN layer, the N-type defect healing layer comprising a first InN layer and an N-type Al layer alternately laminated y Ga 1-y An N layer, wherein the value range of x is 0.1-0.6, and the value range of y is 0.1-0.6;
depositing a second insertion layer on the multiple quantum well layer, comprising the steps of:
sequentially depositing a second MgN three-dimensional layer, a P-type three-dimensional merging layer and a P-type defect healing layer on the multiple quantum well layer, wherein the P-type three-dimensional merging layer comprises alternately laminated Al a Ga 1-a An N layer and a P-type GaN layer, wherein the P-type defect healing layer comprises a second InN layer and a P-type Al layer which are alternately laminated b Ga 1-b And an N layer, wherein the value range of a is 0.1-0.6, and the value range of b is 0.1-0.6.
8. The method for preparing the deep ultraviolet light emitting diode epitaxial wafer of claim 7, wherein sequentially depositing a first MgN three-dimensional layer on the N-type AlGaN layer or sequentially depositing a second MgN three-dimensional layer on the multiple quantum well layer comprises the steps of:
controlling the temperature of the reaction chamber to be 700-800 ℃, and introducing N 2 And (3) introducing a Mg source and an N source as carrier gas, wherein the Mg source is introduced in a pulse manner, so as to finish deposition.
9. The method for preparing the deep ultraviolet light-emitting diode epitaxial wafer according to claim 7, wherein the growth temperature of the N-type three-dimensional merging layer is 1030-1070 ℃;
the growth temperature of the P-type three-dimensional merging layer is 1030-1070 ℃;
the growth temperature of the first InN layer is 900-1000 ℃;
the N type Al y Ga 1-y The temperature of the N layer is 1100-1200 ℃;
the growth temperature of the second InN layer is 1000-1050 ℃;
the P type Al b Ga 1-b The growth temperature of the N layer is 1100-1200 ℃.
10. An LED comprising the deep ultraviolet light emitting diode epitaxial wafer according to any one of claims 1to 6.
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