CN113764555A - AlN ultraviolet light-emitting diode based on nano-pattern insertion layer and preparation method thereof - Google Patents

AlN ultraviolet light-emitting diode based on nano-pattern insertion layer and preparation method thereof Download PDF

Info

Publication number
CN113764555A
CN113764555A CN202110859939.3A CN202110859939A CN113764555A CN 113764555 A CN113764555 A CN 113764555A CN 202110859939 A CN202110859939 A CN 202110859939A CN 113764555 A CN113764555 A CN 113764555A
Authority
CN
China
Prior art keywords
layer
aln
reaction chamber
type
flow
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110859939.3A
Other languages
Chinese (zh)
Other versions
CN113764555B (en
Inventor
许晟瑞
吴前龙
贠博祥
陶鸿昌
许文强
范晓萌
张雅超
张进成
郝跃
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhu Research Institute of Xidian University
Original Assignee
Wuhu Research Institute of Xidian University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhu Research Institute of Xidian University filed Critical Wuhu Research Institute of Xidian University
Priority to CN202110859939.3A priority Critical patent/CN113764555B/en
Publication of CN113764555A publication Critical patent/CN113764555A/en
Application granted granted Critical
Publication of CN113764555B publication Critical patent/CN113764555B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/10—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a light reflecting structure, e.g. semiconductor Bragg reflector
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0062—Processes for devices with an active region comprising only III-V compounds
    • H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
    • H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/20—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate
    • 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

Landscapes

  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Led Devices (AREA)

Abstract

The invention discloses an AlN ultraviolet light-emitting diode based on a nano-graph insertion layer and a preparation method thereof, wherein the AlN ultraviolet light-emitting diode comprises the following components from bottom to top: patterned sapphire substrate, AlN nanopattern insertion layer, AlN regrowth layer, n-type AlN layer, AlxGa1‑xN/AlyGa1‑yN multi-quantum well layer and AlzGa1‑zThe N-type GaN-based solar cell comprises an N electron blocking layer, a p-type AlN layer, a p-type GaN contact layer, a p-type electrode and an N-type electrode; the AlN nanopattern insertion layer is covered with a first Ag reflecting layer and a second Ag reflecting layer. The invention can overcome the defects of high dislocation density, low light extraction efficiency and light output power in the heteroepitaxial AlGaN/AlN-based light-emitting diodeLow problem, and high performance AlN ultraviolet LED.

Description

AlN ultraviolet light-emitting diode based on nano-pattern insertion layer and preparation method thereof
Technical Field
The invention belongs to the technical field of microelectronics, and particularly relates to an AlN ultraviolet light-emitting diode based on a graph insertion layer and a preparation method thereof.
Background
An ultraviolet Light Emitting Diode (LED) is one of the most widely used Light Emitting devices today, and for a traditional ultraviolet Light source, for example: mercury lamps, long wavelength uv lamps, metal halide lamps, etc., which have a number of inherent drawbacks that are difficult to overcome, such as: harmful substances, environmental pollution, low efficiency, high energy consumption, short life, single wavelength, etc., so the international research on novel ultraviolet light sources is also pushed on the schedule one after another and becomes one of the hot spots concerned by each country in the semiconductor field. Because AlN belongs to a direct band gap ultra-wideband semiconductor material, the ultraviolet LED based on AlGaN has the advantages that the traditional ultraviolet light source does not have, such as no pollution, low energy consumption, long service life, adjustable wavelength and the like, and therefore AlN becomes the most ideal material for obtaining ultraviolet and deep ultraviolet light sources in a new era.
In recent years, research on AlGaN/AlN-based ultraviolet LEDs is rapidly developed, and the performance of AlN ultraviolet LED devices can be effectively improved by applying the technologies of epitaxial lateral overgrowth, patterned substrates, face-to-face annealing and the like. However, the performance of this level is far from the expected value, and many problems have not been solved. Such as the following aspects:
first, AlN and sapphire substratesThe lattice mismatch and the thermal expansion coefficient difference between the two are large, so that the dislocation density in the epitaxial AlN crystal is high (1010 cm)-2) A large amount of dislocations penetrate and grow to the active region, and as a non-radiative recombination center, Internal Quantum Efficiency (IQE) is reduced, so that the luminous Efficiency of the LED device is greatly reduced.
Secondly, the difference between the refractive index of the AlN material and air is large, and light from the quantum well is totally reflected inside the LED device, resulting in low Light Extraction Efficiency (LEE), and thus, a reduction in light emission efficiency.
And thirdly, spontaneous polarization, piezoelectric polarization and quantum stark limiting effect exist in the epitaxial layer crystal growing along the C surface, and the energy band of the multiple quantum well is distorted by the generated internal polarization electric field, so that the wave functions of electrons and holes are further separated, and the radiation recombination probability is reduced.
Fourth, AlN doping (especially P-type doping) is extremely difficult, i.e., the number of available carriers inside the LED is limited, affecting the probability of electron and hole recombination.
Based on the above problems and the superposition of other factors, the luminous efficiency of the AlN ultraviolet LED device is less than 10%, and the application is limited.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an AlN ultraviolet light-emitting diode based on a nano-pattern insertion layer and a preparation method thereof. The technical problem to be solved by the invention is realized by the following technical scheme:
an AlN ultraviolet light-emitting diode based on a nanometer pattern insertion layer, the AlN ultraviolet light-emitting diode comprises from bottom to top: patterned sapphire substrate, AlN nanopattern insertion layer, AlN regrowth layer, n-type AlN layer, AlxGa1-xN/AlyGa1-yN multi-quantum well layer and AlzGa1-zThe N-type GaN-based solar cell comprises an N electron blocking layer, a p-type AlN layer, a p-type GaN contact layer, a p-type electrode and an N-type electrode; the surface of the AlN nano-pattern insertion layer is covered with an Ag first light reflecting layer and an Ag second light reflecting layer.
In one embodiment of the present invention, the patterned sapphire substrate is a C-plane patterned sapphire substrate; the AlN nanopattern insertion layer is 2-15um thick.
In one embodiment of the present invention, the Ag first light reflecting layer and the Ag second light reflecting layer are metal materials; the thickness of the Ag first reflecting layer and the Ag second reflecting layer is 10-500 nm; the Ag first light reflecting layer covers the top surface of the convex region of the AlN nanopattern insertion layer, and the Ag second light reflecting layer covers the bottom surface of the concave region of the AlN nanopattern insertion layer.
The invention has the beneficial effects that:
1. the invention combines the double-reflection layer structure based on the AlN nano-pattern insertion layer, can inhibit a large amount of dislocation from upwards propagating and growing from the lower layer structure, thereby reducing the dislocation density in the upper layer structure, achieving the purposes of improving the crystal quality and further enhancing the internal quantum efficiency.
2. The AlN nano-pattern insertion layer is combined with the double-reflection layer structure, and can be used as an internal light blocking layer and a reflection center, so that light can be prevented from being transmitted to the back of the light-emitting diode on one hand, more light can be reflected to a light-emitting window above the light-emitting diode on the other hand, the light-emitting probability is improved, and the light extraction efficiency is improved.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic structural diagram of an AlN ultraviolet light-emitting diode based on a nanopattern insertion layer according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of a method for preparing an AlN ultraviolet light-emitting diode based on a nanopattern insertion layer according to an embodiment of the invention;
fig. 3 is a schematic diagram of a process for preparing an AlN ultraviolet led based on a nanopattern insertion layer according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example one
Referring to fig. 1, fig. 1 is a schematic structural diagram of an AlN ultraviolet led based on a nanopattern insertion layer according to an embodiment of the present invention, where the AlN ultraviolet led includes, from bottom to top: patterned sapphire substrate, AlN nanopattern insertion layer, AlN regrowth layer, n-type AlN layer, AlxGa1-xN/AlyGa1-yN multi-quantum well layer and AlzGa1-zThe N-type GaN-based solar cell comprises an N electron blocking layer, a p-type AlN layer, a p-type GaN contact layer, a p-type electrode and an N-type electrode; the surface of the AlN nano-pattern insertion layer is covered with an Ag first light reflecting layer and an Ag second light reflecting layer.
Optionally, the patterned sapphire substrate is a C-plane patterned sapphire substrate; the AlN nanopattern insertion layer is 2-15um thick.
Optionally, the first Ag reflective layer and the second Ag reflective layer are made of a metal material; the thickness of the Ag first reflecting layer and the Ag second reflecting layer is 10-500 nm; the Ag first light reflecting layer covers the top surface of the convex region of the AlN nanopattern insertion layer, and the Ag second light reflecting layer covers the bottom surface of the concave region of the AlN nanopattern insertion layer.
Optionally, in the AlxGa1-xN/AlyGa1-yIn the N multi-quantum well layer, the number of cycles of the multi-quantum well is 5-20, and the Al isxGa1-xN and AlyGa1-yN is an alternate structure 1, wherein one layer of AlxGa1-xA layer of Al to which N is bondedyGa1-yN is a multiple quantum well period.
Optionally, each layer of AlxGa1-xN is 5-30nm thick, and each layer of AlyGa1-yThe thickness of N is 10-40 nm.
Optionally, the AlxGa1-xN/AlyGa1-yIn the N multi-quantum well layer, the value range of x is 0.01-0.8, and the value range of y is 0.1-1.
Optionally, the AlN regrowth layer has a thickness of 2-15-nm; the thickness of the n-type AlN layer is 3-20 nm.
Optionally, the AlzGa1-zThe thickness of the N electron blocking layer is 10-200nm, wherein the value range of the Al component z is 0.5-1.
In conclusion, the invention has the beneficial effects that:
1. the invention combines the double-reflection layer structure based on the AlN nano-pattern insertion layer, can inhibit a large amount of dislocation from upwards propagating and growing from the lower layer structure, thereby reducing the dislocation density in the upper layer structure, achieving the purposes of improving the crystal quality and further enhancing the internal quantum efficiency.
2. The AlN nano-pattern insertion layer is combined with the double-reflection layer structure, and can be used as an internal light blocking layer and a reflection center, so that light can be prevented from being transmitted to the back of the light-emitting diode on one hand, more light can be reflected to a light-emitting window above the light-emitting diode on the other hand, the light-emitting probability is improved, the light extraction efficiency is improved, the light output power is improved, and the high-performance AlN ultraviolet light-emitting diode is obtained.
Example two
Referring to fig. 2, fig. 2 is a schematic flow chart of a method for preparing an AlN ultraviolet led based on a nanopattern insertion layer according to an embodiment of the present invention, where the method includes:
step 1: and carrying out heating nitridation treatment on the patterned sapphire substrate in a preset reaction chamber based on pretreatment parameters, wherein the pretreatment parameters comprise a preheating treatment parameter and a nitridation treatment parameter.
Optionally, the patterned sapphire substrate is a C-plane patterned sapphire substrate.
Optionally, step 1 includes:
step 1-1: and cleaning the pattern sapphire substrate.
Step 1-2: and carrying out preheating treatment on the cleaned graph sapphire substrate based on preheating treatment parameters, wherein the preheating treatment parameters comprise the vacuum degree of a reaction chamber, the first hydrogen flow, the first pressure of the reaction chamber, the heating temperature of a substrate target and the holding time of the heating temperature of the substrate target.
Step 1-3: and performing nitridation treatment on the graph sapphire substrate subjected to the preheating treatment based on nitridation treatment parameters, wherein the nitridation treatment parameters comprise a first temperature of the reaction chamber, a first ammonia gas flow and ammonia gas introduction time.
The present invention enables the preparation of AlN uv-leds using a Metal-organic Chemical Vapor Deposition (MOCVD) reaction chamber. Specifically, the MOCVD reaction chamber is pre-configured with the pre-treatment parameters, and the cleaned patterned sapphire substrate is placed in the MOCVD reaction chamber to be subjected to pre-heating treatment and nitriding treatment.
The pre-heat treatment parameter and the nitridation treatment parameter are set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto. In the preheating treatment, the degree of vacuum of the reaction chamber is usually 3X 10- 2The first pressure of the reaction chamber is 25Torr, the target heating temperature of the substrate is 900 ℃, the time for keeping the target heating temperature of the substrate is ten minutes, and in the nitriding treatment, the first temperature of the reaction chamber is 1000 ℃, the first ammonia gas flow is 3500sccm and the ammonia gas introduction time is 3 minutes.
For example, the degree of vacuum of the reaction chamber is adjusted to 3X 10-2Torr, hydrogen is introduced into the MOCVD reaction chamber, when the pressure of the reaction chamber is increased to 25Torr, the temperature of the substrate is heated to 900 ℃, the temperature is kept for 10 minutes, and the preheating treatment of the substrate is completed; the temperature of the MOCVD reaction chamber is raised to 1000 ℃, then ammonia gas with the flow rate of 3500sccm is introduced, the process lasts for 3 minutes, and the nitridation treatment of the substrate is completed.
Step 2: and based on a first growth parameter, growing an AlN nano-pattern insertion layer on the pattern sapphire substrate after the nitridation treatment, wherein the first growth parameter comprises an AlN layer growth parameter, a first thermal annealing parameter and an etching parameter.
The first growth parameter is set by a person skilled in the art according to business needs, and it is understood that the present invention is not limited in this regard.
Optionally, step 2 includes:
step 2-1: and growing an AlN layer on the graph sapphire substrate after the nitridation treatment based on the AlN layer growth parameters, wherein the AlN layer growth parameters comprise a second temperature of the reaction chamber, a second pressure of the reaction chamber, a second ammonia flow and a first aluminum source flow.
Step 2-2: and carrying out thermal annealing treatment on the AlN layer based on first thermal annealing parameters, wherein the first thermal annealing parameters comprise a first thermal annealing temperature and a first thermal annealing time length.
Step 2-3: and etching the AlN layer subjected to the thermal annealing treatment based on etching parameters, wherein the etching parameters comprise the proportion of boron trichloride and the proportion of chlorine gas flow, the third pressure of the reaction chamber, the power of the reaction chamber and the etching time.
Step 2-4: and removing Ni metal on the surface of the etched AlN layer based on an acid solution corrosion process to obtain the AlN nano-pattern insertion layer.
Typically, the second temperature of the reaction chamber is 1050 ℃, the second pressure of the reaction chamber is 20Torr, the flow rate of the second ammonia gas is 3000sccm, and the flow rate of the first aluminum source is 40sccm, and the first thermal annealing temperature is 800 ℃ and the first thermal annealing time is 2 minutes.
Such as: placing the nitrided c-plane graphic sapphire substrate into an MOCVD reaction chamber, raising the temperature of the reaction chamber to 1050 ℃, adjusting the pressure to 20Torr, introducing ammonia gas with the flow of 3000sccm and an aluminum source with the flow of 40sccm, and growing an AlN layer with the thickness of 3 um; depositing a layer of Ni metal with the thickness of 3nm on the AlN layer by using an electron beam evaporation process; annealing for 2 minutes at 800 ℃ in a nitrogen atmosphere by using a rapid thermal annealing process; using reactive ion etching process, introducing etching gas boron trichloride BCl into a reaction chamber3And chlorine Cl2The ratio is 30: 75, etching the AlN subjected to annealing for 1 minute under the pressure of 25mTorr and the power of 150W, wherein the etching thickness is 200 nm; and removing the Ni metal on the surface of the AlN by using an acid solution etching process.
And step 3: and covering the surface of the AlN nano-pattern insertion layer with an Ag first light reflecting layer and an Ag second light reflecting layer.
The invention can use electron beam evaporation technology to deposit a 10nm thick Ag reflecting layer on the top surface and the bottom plane area of the AlN insert layer pattern.
And 4, step 4: growing an AlN regrowth layer on the Ag first reflecting layer and the Ag second reflecting layer based on second growth parameters, wherein the second growth parameters comprise a third temperature of the reaction chamber, a fourth pressure of the reaction chamber, a third ammonia flow and a second aluminum source flow;
the second growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Typically, the third temperature of the reaction chamber is 1000 deg.C, the fourth pressure of the reaction chamber is 20Torr, the third ammonia gas flow rate, 3000sccm, and the second aluminum source flow rate is 40sccm, as follows: and (3) using an MOCVD process, raising the temperature of the reaction chamber to 1000 ℃, adjusting the pressure to 20Torr, introducing ammonia gas with the flow of 3000sccm and an aluminum source with the flow of 40sccm, and growing an AlN regrowth layer with the thickness of 3um on the reflecting layer.
And 5: growing an n-type AlN layer on the AlN regrowth layer based on third growth parameters, the third growth parameters including a reaction chamber fourth temperature, a reaction chamber fifth pressure, a fourth ammonia flow, a third aluminum source flow, and a silicon source flow.
The third growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Typically, the fourth temperature of the reaction chamber is 1000 ℃, the fifth pressure of the reaction chamber is 30Torr, the flow rate of the fourth ammonia gas is 3000sccm, the flow rate of the third aluminum source is 40sccm, and the flow rate of the silicon source is 200sccm, such as: by using the MOCVD process, the temperature of the reaction chamber is raised to 1000 ℃, the pressure is increased to 30Torr, ammonia gas with the flow rate of 3000sccm, an aluminum source with the flow rate of 40sccm and a silicon source with the flow rate of 200sccm are introduced, and an n-type AlN layer with the thickness of 3um is grown on the regrown AlN layer.
Step 6: growing Al on the n-type AlN layer based on a fourth growth parameterxGa1-xN/AlyGa1-yAnd the fourth growth parameter comprises a fifth temperature of the reaction chamber, a sixth pressure of the reaction chamber, a growth period, a nitrogen source flow, a first gallium source flow and a fourth aluminum source flow.
The fourth growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Typically, the fifth temperature of the chamber is 1000 deg.C, the sixth pressure of the chamber is 20Torr, the growth period is 5 cycles, and the nitrogen source flow is 3000 sccm.
Such as: using MOCVD process, the chamber temperature was raised to 1000 deg.C and the pressure was adjusted to 20Torr to grow 5 cycles of Al on n-type AlN0.55Ga0.45N/Al0.7Ga0.3And an N quantum well. Monolayer of Al per period0.55Ga0.45N well layer and Al0.7Ga0.3The thickness of the N barrier layer is 10nm and 30nm respectively, wherein the flow of the nitrogen source is kept at 3000sccm in the growth process, and Al is grown0.55Ga0.45When the N well layer is formed, the gallium source flow is kept to be 80sccm, and the aluminum source flow is kept to be 120 sccm; in growing Al0.7Ga0.3And in the N barrier layer, the gallium source flow is kept to be 47sccm, and the aluminum source flow is kept to be 200 sccm.
And 7: based on a fifth growth parameter, in the AlxGa1-xN/AlyGa1-yGrowing Al on N multi-quantum well layerzGa1-zAnd the fifth growth parameter comprises a sixth temperature of the reaction chamber, a seventh pressure of the reaction chamber, a fifth ammonia flow, a second gallium source flow and a fifth aluminum source flow.
The fifth growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Typically, the sixth temperature of the reaction chamber is 1000 ℃, the seventh pressure of the reaction chamber is 20Torr, the flow rate of the fifth ammonia gas is 1500sccm, the flow rate of the second gallium source is 40sccm, and the flow rate of the fifth aluminum source is 180sccm, such as:
using MOCVD process, the temperature of the reaction chamber is raised to 1000 ℃, the pressure is adjusted to 20Torr, and ammonia gas with the flow of 1500sccm, a gallium source with the flow of 40sccm and an aluminum source with the flow of 180sccm are introduced into AlxGa1-xN/AlyGa1-yGrowing Al with the thickness of 20nm on the N multi-quantum well0.8Ga0.2An N electron blocking layer.
And 8: based on the sixth growth parameter, in the AlzGa1-zGrowing a p-type AlN layer on the N-electron blocking layer, wherein the sixth growth parameter comprisesA seventh temperature of the reaction chamber, an eighth pressure of the reaction chamber, a sixth ammonia gas flow, a sixth aluminum source flow and a magnesium source flow.
The sixth growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Typically, the seventh temperature of the reaction chamber is 1050 deg.C, the eighth pressure of the reaction chamber is 20Torr, the sixth ammonia gas flow is 3000sccm, the sixth aluminum source flow is 40sccm, the magnesium source flow is 500sccm, as follows: using MOCVD process, the temperature of the reaction chamber is raised to 1050 ℃, the pressure is adjusted to 20Torr, ammonia gas with the flow of 3000sccm, aluminum source with the flow of 40sccm and magnesium source with the flow of 500sccm are introduced into AlzGa1-zAnd growing a p-type AlN layer with the thickness of 100nm on the N electron blocking layer.
And step 9: growing a p-type GaN layer on the p-type AlN layer based on a seventh growth parameter, wherein the seventh growth parameter comprises a GaN layer growth parameter and a second thermal annealing parameter.
The seventh growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Optionally, step 9 includes:
step 9-1: and growing a p-type GaN layer on the p-type AlN layer based on the GaN layer growth parameters, wherein the GaN layer growth parameters comprise the eighth temperature of the reaction chamber, the ninth pressure of the reaction chamber, the seventh ammonia gas flow, the third gallium source flow, the second magnesium source flow, the ninth temperature of the reaction chamber and the second hydrogen gas flow.
Step 9-2: and carrying out thermal annealing treatment on the p-type GaN layer based on second thermal annealing parameters, wherein the second thermal annealing parameters comprise a second thermal annealing temperature and a second thermal annealing time length.
Usually the eighth temperature of the reaction chamber is 980 ℃, the ninth pressure of the reaction chamber is 20Torr, the flow of the seventh ammonia gas is 2500sccm, the flow of the third gallium source is 150sccm, and the flow of the second magnesium source is 100 sccm; the second thermal annealing temperature is 850 ℃ and the second thermal annealing time is 10 min. If an MOCVD process is used, the temperature of the reaction chamber is raised to 980 ℃, the pressure is adjusted to 20Torr, ammonia gas with the flow of 2500sccm, a gallium source with the flow of 150sccm and a magnesium source with the flow of 100sccm are introduced, and a p-type GaN layer with the thickness of 100nm grows on p-type AlN; then the temperature of the reaction chamber is maintained at 850 ℃, and annealing is carried out for 10min under the hydrogen atmosphere.
Step 10: and respectively manufacturing an n-type electrode and a p-type electrode on the n-type AlN layer and the p-type GaN layer.
Optionally, the step 10 includes:
based on the sputtering process, an n-type electrode is sputtered on the n-type AlN layer, and a p-type electrode is sputtered on the p-type GaN layer.
Based on the parameters provided by the second embodiment, the ultraviolet light-emitting diode with the light-emitting wavelength of 265nm can be obtained. Referring to fig. 3, fig. 3 is a schematic diagram of a process for preparing an AlN ultraviolet led based on a nanopattern insertion layer according to an embodiment of the present invention.
In conclusion, the invention has the beneficial effects that:
1. the invention combines the double-reflection layer structure based on the AlN nano-pattern insertion layer, can inhibit a large amount of dislocation from upwards propagating and growing from the lower layer structure, thereby reducing the dislocation density in the upper layer structure, achieving the purposes of improving the crystal quality and further enhancing the internal quantum efficiency.
2. The AlN nano-pattern insertion layer is combined with the double-reflection layer structure, and can be used as an internal light blocking layer and a reflection center, so that light can be prevented from being transmitted to the back of the light-emitting diode on one hand, more light can be reflected to a light-emitting window above the light-emitting diode on the other hand, the light-emitting probability is improved, the light extraction efficiency is improved, the light output power is improved, and the high-performance AlN ultraviolet light-emitting diode is obtained.
EXAMPLE III
Step 1: and carrying out heating nitridation treatment on the patterned sapphire substrate in a preset reaction chamber based on pretreatment parameters, wherein the pretreatment parameters comprise a preheating treatment parameter and a nitridation treatment parameter.
Step 2: and based on a first growth parameter, growing an AlN nano-pattern insertion layer on the pattern sapphire substrate after the nitridation treatment, wherein the first growth parameter comprises an AlN layer growth parameter, a first thermal annealing parameter and an etching parameter.
The first growth parameter is set by a person skilled in the art according to business needs, and it is understood that the present invention is not limited in this regard.
Optionally, step 2 includes:
step 2-1: and growing an AlN layer on the graph sapphire substrate after the nitridation treatment based on the AlN layer growth parameters, wherein the AlN layer growth parameters comprise a second temperature of the reaction chamber, a second pressure of the reaction chamber, a second ammonia flow and a first aluminum source flow.
Step 2-2: and carrying out thermal annealing treatment on the AlN layer based on first thermal annealing parameters, wherein the first thermal annealing parameters comprise a first thermal annealing temperature and a first thermal annealing time length.
Step 2-3: and etching the AlN layer subjected to the thermal annealing treatment based on etching parameters, wherein the etching parameters comprise the proportion of boron trichloride and the proportion of chlorine gas flow, the third pressure of the reaction chamber, the power of the reaction chamber and the etching time.
Step 2-4: and removing Ni metal on the surface of the etched AlN layer based on an acid solution corrosion process to obtain the AlN nano-pattern insertion layer.
Such as: placing the nitrided c-plane graphic sapphire substrate into an MOCVD reaction chamber, raising the temperature of the reaction chamber to 1100 ℃, stressing to 30Torr, introducing ammonia gas with the flow of 4000sccm and an aluminum source with the flow of 50sccm, and growing an AlN layer with the thickness of 5 um; depositing a layer of Ni metal with the thickness of 5nm on the AlN layer by using an electron beam evaporation process; annealing for 2 minutes at 850 ℃ in a nitrogen atmosphere by using a rapid thermal annealing process; using a reactive ion etching process, introducing an etching gas BCl into a reaction chamber3And Cl2The ratio is 40: 90, etching the AlN subjected to annealing for 3 minutes under the pressure of 30mTorr and the power of 150W, wherein the etching thickness is 500 nm; and removing the Ni metal on the surface of the AlN by using an acid solution etching process.
And step 3: and covering the surface of the AlN nano-pattern insertion layer with an Ag first light reflecting layer and an Ag second light reflecting layer.
In this embodiment, a 20nm thick reflective layer of Ag can be deposited on the top and bottom planar regions of the AlN insert pattern using an electron beam evaporation process.
And 4, step 4: and growing an AlN regrowth layer on the Ag first reflecting layer and the Ag second reflecting layer based on second growth parameters, wherein the second growth parameters comprise a third temperature of the reaction chamber, a fourth pressure of the reaction chamber, a third ammonia gas flow and a second aluminum source flow.
The second growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: by using the MOCVD process, the temperature of the reaction chamber is raised to 1050 ℃, the pressure is enhanced to 30Torr, ammonia gas with the flow rate of 3500sccm and an aluminum source with the flow rate of 50sccm are introduced, and an AlN regrowth layer with the thickness of 5um is grown on the reflecting layer.
And 5: growing an n-type AlN layer on the AlN regrowth layer based on third growth parameters, the third growth parameters including a reaction chamber fourth temperature, a reaction chamber fifth pressure, a fourth ammonia flow, a third aluminum source flow, and a silicon source flow.
The third growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: by using the MOCVD process, the temperature of the reaction chamber is raised to 1050 ℃, the pressure is increased to 50Torr, ammonia gas with the flow rate of 3500sccm, an aluminum source with the flow rate of 50sccm and a silicon source with the flow rate of 300sccm are introduced, and an n-type AlN layer with the thickness of 7um is grown on the regrown AlN layer.
Step 6: growing Al on the n-type AlN layer based on a fourth growth parameterxGa1-xN/AlyGa1-yAnd the fourth growth parameter comprises a fifth temperature of the reaction chamber, a sixth pressure of the reaction chamber, a growth period, a nitrogen source flow, a first gallium source flow and a fourth aluminum source flow.
The fourth growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: by using MOCVD process, the temperature of the reaction chamber is raised to 1050 ℃ and the pressure is adjusted to 30Torrr, growth of 8 cycles of Al on n-type AlN0.29Ga0.71N/Al0.55Ga0.45And an N quantum well. Monolayer of Al per period0.29Ga0.71N well layer and Al0.55Ga0.45The thickness of the N barrier layer is 15nm and 25nm respectively, wherein the flow of the nitrogen source is kept at 1500sccm in the growth process, and Al is grown0.29Ga0.71When the N well layer is formed, the flow rate of a gallium source is kept to be 45sccm, and the flow rate of an aluminum source is kept to be 145 sccm; in the growth of Al0.55Ga0.45And in the N barrier layer, the gallium source flow is kept to be 55sccm, and the aluminum source flow is kept to be 190 sccm.
And 7: based on a fifth growth parameter, in the AlxGa1-xN/AlyGa1-yGrowing Al on N multi-quantum well layerzGa1-zAnd the fifth growth parameter comprises a sixth temperature of the reaction chamber, a seventh pressure of the reaction chamber, a fifth ammonia flow, a second gallium source flow and a fifth aluminum source flow.
The fifth growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: using MOCVD process, the temperature of the reaction chamber is raised to 1100 ℃, the pressure is adjusted to 40Torr, ammonia gas with the flow of 2000sccm, a gallium source with the flow of 35sccm and an aluminum source with the flow of 150sccm are introduced into the reaction chamber, and Al is added into the reaction chamberxGa1-xN/AlyGa1-yGrowing Al with the thickness of 30nm on the N multi-quantum well0.7Ga0.3An N electron blocking layer.
And 8: based on the sixth growth parameter, in the AlzGa1-zAnd growing a p-type AlN layer on the N electron blocking layer, wherein the sixth growth parameter comprises a seventh temperature of the reaction chamber, an eighth pressure of the reaction chamber, a sixth ammonia gas flow, a sixth aluminum source flow and a magnesium source flow.
The sixth growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: using MOCVD process, the temperature of the reaction chamber is raised to 1100 ℃, the pressure is emphasized to 30Torr, and ammonia gas with the flow rate of 4000sccm and the flow rate of 50sccm are introducedAluminum source of sccm, magnesium source at a flow rate of 600sccm, in AlzGa1-zAnd growing a p-type AlN layer with the thickness of 120nm on the N electron blocking layer.
And step 9: growing a p-type GaN layer on the p-type AlN layer based on a seventh growth parameter, wherein the seventh growth parameter comprises a GaN layer growth parameter and a second thermal annealing parameter.
The seventh growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Optionally, step 9 includes:
step 9-1: and growing a p-type GaN layer on the p-type AlN layer based on the GaN layer growth parameters, wherein the GaN layer growth parameters comprise the eighth temperature of the reaction chamber, the ninth pressure of the reaction chamber, the seventh ammonia gas flow, the third gallium source flow, the second magnesium source flow, the ninth temperature of the reaction chamber and the second hydrogen gas flow.
Step 9-2: and carrying out thermal annealing treatment on the p-type GaN layer based on second thermal annealing parameters, wherein the second thermal annealing parameters comprise a second thermal annealing temperature and a second thermal annealing time length.
Such as: by using the MOCVD process, the temperature of the reaction chamber is raised to 950 ℃, the pressure is emphasized to 50Torr, ammonia gas with the flow rate of 2000sccm, a gallium source with the flow rate of 150sccm and a magnesium source with the flow rate of 150sccm are introduced, a p-type GaN layer with the thickness of 80nm is grown on the p-type AlN, and then the temperature of the reaction chamber is maintained at 850 ℃, and annealing is carried out for 8min in a hydrogen atmosphere.
Step 10: and respectively manufacturing an n-type electrode and a p-type electrode on the n-type AlN layer and the p-type GaN layer.
Optionally, the step 10 includes:
based on the sputtering process, an n-type electrode is sputtered on the n-type AlN layer, and a p-type electrode is sputtered on the p-type GaN layer.
Based on the parameters provided by the third embodiment, the ultraviolet light-emitting diode with the light-emitting wavelength of 310nm can be obtained.
Example four
Step 1: and carrying out heating nitridation treatment on the patterned sapphire substrate in a preset reaction chamber based on pretreatment parameters, wherein the pretreatment parameters comprise a preheating treatment parameter and a nitridation treatment parameter.
Step 2: and based on a first growth parameter, growing an AlN nano-pattern insertion layer on the pattern sapphire substrate after the nitridation treatment, wherein the first growth parameter comprises an AlN layer growth parameter, a first thermal annealing parameter and an etching parameter.
The first growth parameter is set by a person skilled in the art according to business needs, and it is understood that the present invention is not limited in this regard.
Optionally, step 2 includes:
step 2-1: and growing an AlN layer on the graph sapphire substrate after the nitridation treatment based on the AlN layer growth parameters, wherein the AlN layer growth parameters comprise a second temperature of the reaction chamber, a second pressure of the reaction chamber, a second ammonia flow and a first aluminum source flow.
Step 2-2: and carrying out thermal annealing treatment on the AlN layer based on first thermal annealing parameters, wherein the first thermal annealing parameters comprise a first thermal annealing temperature and a first thermal annealing time length.
Step 2-3: and etching the AlN layer subjected to the thermal annealing treatment based on etching parameters, wherein the etching parameters comprise the proportion of boron trichloride and the proportion of chlorine gas flow, the third pressure of the reaction chamber, the power of the reaction chamber and the etching time.
Step 2-4: and removing Ni metal on the surface of the etched AlN layer based on an acid solution corrosion process to obtain the AlN nano-pattern insertion layer.
Such as: placing the nitrided c-plane graphic sapphire substrate into an MOCVD reaction chamber, raising the temperature of the reaction chamber to 1150 ℃, stressing to 50Torr, introducing ammonia gas with the flow of 5000sccm and an aluminum source with the flow of 60sccm, and growing an AlN layer with the thickness of 8 um; depositing a layer of Ni metal with the thickness of 10nm on the AlN layer by using an electron beam evaporation process, and then annealing for 3 minutes by using a rapid thermal annealing process at the temperature of 900 ℃ under the nitrogen atmosphere; using a reactive ion etching process, introducing an etching gas BCl into a reaction chamber3And Cl2The ratio is 40: 100, pressure 50mTorr, power 4Etching the AlN subjected to annealing for 4 minutes at 50W, wherein the etching thickness is 1000 nm; and removing the Ni metal on the surface of the AlN by using an acid solution etching process.
And step 3: and covering the surface of the AlN nano-pattern insertion layer with an Ag first light reflecting layer and an Ag second light reflecting layer.
In this embodiment, an 80nm thick Ag reflective layer can be deposited on the top surface and bottom planar regions of the AlN interposer pattern using an electron beam evaporation process.
And 4, step 4: and growing an AlN regrowth layer on the Ag first reflecting layer and the Ag second reflecting layer based on second growth parameters, wherein the second growth parameters comprise a third temperature of the reaction chamber, a fourth pressure of the reaction chamber, a third ammonia gas flow and a second aluminum source flow.
The second growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: by using the MOCVD process, the temperature of the reaction chamber is raised to 1100 ℃, the pressure is enhanced to 50Torr, ammonia gas with the flow rate of 5000sccm and an aluminum source with the flow rate of 80sccm are introduced, and an AlN regrowth layer with the thickness of 8um is grown on the reflecting layer.
And 5: growing an n-type AlN layer on the AlN regrowth layer based on third growth parameters, the third growth parameters including a reaction chamber fourth temperature, a reaction chamber fifth pressure, a fourth ammonia flow, a third aluminum source flow, and a silicon source flow.
The third growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: and (3) using an MOCVD process, raising the temperature of the reaction chamber to 1100 ℃, adjusting the pressure to 60Torr, introducing ammonia gas with the flow of 4500sccm, an aluminum source with the flow of 80sccm and a silicon source with the flow of 450sccm, and growing an n-type AlN layer with the thickness of 10um on the regrown AlN layer.
Step 6: growing Al on the n-type AlN layer based on a fourth growth parameterxGa1-xN/AlyGa1-yAn N multi-quantum well layer, wherein the fourth growth parameter comprises a fifth temperature of the reaction chamber,And the reaction chamber has a sixth pressure, a growth period, a nitrogen source flow rate, a first gallium source flow rate and a fourth aluminum source flow rate.
The fourth growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: using MOCVD process, the temperature of the reaction chamber is raised to 1200 ℃, the pressure is adjusted to 60Torr, and Al grows on n-type AlN for 15 periods0.7Ga0.3N/Al0.85Ga0.15And an N quantum well. Monolayer of Al per period0.7Ga0.3N well layer and Al0.85Ga0.15The thickness of the N barrier layer is 25nm and 35nm respectively, wherein the flow of the nitrogen source is kept at 1200sccm in the growth process, and Al is grown0.7Ga0.3When the N well layer is formed, the flow rate of a gallium source is kept to be 45sccm, and the flow rate of an aluminum source is kept to be 130 sccm; in growing Al0.85Ga0.15And when the N barrier layer is formed, the flow of an aluminum source is kept at 130sccm, and the flow of a gallium source is kept at 24.
And 7: based on a fifth growth parameter, in the AlxGa1-xN/AlyGa1-yGrowing Al on N multi-quantum well layerzGa1-zAnd the fifth growth parameter comprises a sixth temperature of the reaction chamber, a seventh pressure of the reaction chamber, a fifth ammonia flow, a second gallium source flow and a fifth aluminum source flow.
The fifth growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: by using the MOCVD process, the temperature of the reaction chamber is raised to 1200 ℃, the pressure is adjusted to 60Torr, ammonia gas with the flow of 1200sccm, a gallium source with the flow of 45sccm and an aluminum source with the flow of 130sccm are introduced into AlxGa1-xN/AlyGa1-yGrowing Al with the thickness of 50nm on the N multi-quantum well0.95Ga0.05And blocking N electrons.
And 8: based on the sixth growth parameter, in the AlzGa1-zGrowing a p-type AlN layer on the N electron blocking layer, wherein the sixth growth parameter comprises a seventh temperature of the reaction chamber, an eighth pressure of the reaction chamber, a sixth ammonia gas flow and a sixthSix aluminum source flow rates and magnesium source flow rates.
The sixth growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Such as: using MOCVD process, the temperature of the reaction chamber is raised to 1200 ℃, the pressure is adjusted to 60Torr, ammonia gas with the flow of 1200sccm, an aluminum source with the flow of 30sccm and a magnesium source with the flow of 400sccm are introduced into AlzGa1-zAnd growing a p-type AlN layer with the thickness of 150nm on the N electron blocking layer.
And step 9: growing a p-type GaN layer on the p-type AlN layer based on a seventh growth parameter, wherein the seventh growth parameter comprises a GaN layer growth parameter and a second thermal annealing parameter.
The seventh growth parameter is set by those skilled in the art according to business needs, and it is understood that the present invention is not particularly limited thereto.
Optionally, step 9 includes:
step 9-1: and growing a p-type GaN layer on the p-type AlN layer based on the GaN layer growth parameters, wherein the GaN layer growth parameters comprise the eighth temperature of the reaction chamber, the ninth pressure of the reaction chamber, the seventh ammonia gas flow, the third gallium source flow, the second magnesium source flow, the ninth temperature of the reaction chamber and the second hydrogen gas flow.
Step 9-2: and carrying out thermal annealing treatment on the p-type GaN layer based on second thermal annealing parameters, wherein the second thermal annealing parameters comprise a second thermal annealing temperature and a second thermal annealing time length.
Such as: by using the MOCVD process, the temperature of the reaction chamber is raised to 1000 ℃, the pressure is adjusted to 60Torr, ammonia gas with the flow of 2700sccm, a gallium source with the flow of 160sccm and a magnesium source with the flow of 120sccm are introduced, a p-type GaN layer with the thickness of 150nm is grown on the p-type AlN, then the temperature of the reaction chamber is maintained at 900 ℃, and annealing is carried out for 10min in a hydrogen atmosphere.
Step 10: and respectively manufacturing an n-type electrode and a p-type electrode on the n-type AlN layer and the p-type GaN layer.
Optionally, the step 10 includes:
based on the sputtering process, an n-type electrode is sputtered on the n-type AlN layer, and a p-type electrode is sputtered on the p-type GaN layer.
Based on the parameters provided by the fourth embodiment, the ultraviolet light-emitting diode with the light-emitting wavelength of 241nm can be obtained.
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", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and 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 thus, should not be considered as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by those skilled in the art.
While the present application has been described in connection with various embodiments, other variations to the disclosed embodiments can be understood and effected by those skilled in the art in practicing the claimed application, from a review of the drawings, the disclosure, and the appended claims. In the claims, the word "comprising" does not exclude other elements or steps, and the word "a" or "an" does not exclude a plurality. A single processor or other unit may fulfill the functions of several items recited in the claims. The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measures cannot be used to advantage.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

Claims (10)

1. An AlN ultraviolet light-emitting diode based on a nano-pattern insertion layer, which is characterized by comprising from bottom to top: patterned sapphire substrate, AlN nanopattern insertion layer, AlN regrowth layer, n-type AlN layer, AlxGa1-xN/AlyGa1-yN multiple quantumWell layer and AlzGa1-zThe N-type GaN-based solar cell comprises an N electron blocking layer, a p-type AlN layer, a p-type GaN contact layer, a p-type electrode and an N-type electrode;
the surface of the AlN nano-pattern insertion layer is covered with an Ag first light reflecting layer and an Ag second light reflecting layer.
2. The led of claim 1, wherein said patterned sapphire substrate is a C-plane patterned sapphire substrate; the AlN nanopattern insertion layer is 2-15um thick.
3. The led of claim 1, wherein the first and second Ag light-reflecting layers are metallic; the thickness of the Ag first reflecting layer and the Ag second reflecting layer is 10-500 nm; the Ag first light reflecting layer covers the top surface of the convex region of the AlN nanopattern insertion layer, and the Ag second light reflecting layer covers the bottom surface of the concave region of the AlN nanopattern insertion layer.
4. The LED of claim 1, wherein Al is in the AlxGa1-xN/AlyGa1-yIn the N multi-quantum well layer, the number of cycles of the multi-quantum well is 5-20, and the Al isxGa1-xN and AlyGa1-yN is an alternating structure in which a layer of AlxGa1-xA layer of Al to which N is bondedyGa1-yN is a multiple quantum well period; each layer of AlxGa1-xN is 5-30nm thick, and each layer of AlyGa1-yThe thickness of N is 10-40 nm;
the Al isxGa1-xN/AlyGa1-yIn the N multi-quantum well layer, the value range of x is 0.01-0.8, and the value range of y is 0.1-1.
5. The led of claim 1, wherein said AlN regrowth layer has a thickness of 2-15-nm; the thickness of the n-type AlN layer is 3-20 nm;
the Al iszGa1-zThe thickness of the N electron blocking layer is 10-200nm, wherein the value range of the Al component z is 0.5-1;
the thickness of the p-type AlN layer is 50-500 nm;
the thickness of the p-type GaN layer is 30-200 nm.
6. A preparation method of an AlN ultraviolet light-emitting diode based on a nano-pattern insertion layer is characterized by comprising the following steps:
step 1: carrying out heating nitridation treatment on the patterned sapphire substrate in a preset reaction chamber based on pretreatment parameters, wherein the pretreatment parameters comprise a preheating treatment parameter and a nitridation treatment parameter;
step 2: growing an AlN nano-pattern insertion layer on the pattern sapphire substrate after the nitridation treatment based on a first growth parameter, wherein the first growth parameter comprises an AlN layer growth parameter, a first thermal annealing parameter and an etching parameter;
and step 3: covering an Ag first light reflecting layer and an Ag second light reflecting layer on the surface of the AlN nano-pattern inserting layer;
and 4, step 4: growing an AlN regrowth layer on the Ag first reflecting layer and the Ag second reflecting layer based on second growth parameters, wherein the second growth parameters comprise a third temperature of the reaction chamber, a fourth pressure of the reaction chamber, a third ammonia flow and a second aluminum source flow;
and 5: growing an n-type AlN layer on the AlN regrowth layer based on third growth parameters, the third growth parameters including a fourth temperature of the reaction chamber, a fifth pressure of the reaction chamber, a fourth ammonia flow, a third aluminum source flow, and a silicon source flow;
step 6: growing Al on the n-type AlN layer based on a fourth growth parameterxGa1-xN/AlyGa1-yThe N multi-quantum well layer, wherein the fourth growth parameter comprises a fifth temperature of the reaction chamber, a sixth pressure of the reaction chamber, a growth period, a nitrogen source flow rate, a first gallium source flow rate and a fourth aluminum source flow rate;
and 7: based on a fifth growth parameter, in the AlxGa1-xN/AlyGa1-yGrowing Al on N multi-quantum well layerzGa1-zThe N electron blocking layer, wherein the fifth growth parameter comprises a sixth temperature of the reaction chamber, a seventh pressure of the reaction chamber, a fifth ammonia flow, a second gallium source flow and a fifth aluminum source flow;
and 8: based on the sixth growth parameter, in the AlzGa1-zGrowing a p-type AlN layer on the N electron blocking layer, wherein the sixth growth parameter comprises a seventh temperature of the reaction chamber, an eighth pressure of the reaction chamber, a sixth ammonia flow, a sixth aluminum source flow and a magnesium source flow;
and step 9: growing a p-type GaN layer on the p-type AlN layer based on a seventh growth parameter, wherein the seventh growth parameter comprises a GaN layer growth parameter and a second thermal annealing parameter.
Step 10: and respectively manufacturing an n-type electrode and a p-type electrode on the n-type AlN layer and the p-type GaN layer.
7. The method of claim 6, wherein the patterned sapphire substrate is a C-plane patterned sapphire substrate, and step 1 comprises:
step 1-1: cleaning the graphic sapphire substrate;
step 1-2: carrying out preheating treatment on the cleaned graph sapphire substrate based on preheating treatment parameters, wherein the preheating treatment parameters comprise the vacuum degree of a reaction chamber, the flow of first hydrogen, the first pressure of the reaction chamber, the heating temperature of a substrate target and the holding time of the heating temperature of the substrate target;
step 1-3: and performing nitridation treatment on the graph sapphire substrate subjected to the preheating treatment based on nitridation treatment parameters, wherein the nitridation treatment parameters comprise a first temperature of the reaction chamber, a first ammonia gas flow and ammonia gas introduction time.
8. The method of claim 6, wherein the step 2 comprises:
step 2-1: growing an AlN layer on the graph sapphire substrate after the nitridation treatment based on AlN layer growth parameters, wherein the AlN layer growth parameters comprise a second temperature of the reaction chamber, a second pressure of the reaction chamber, a second ammonia flow and a first aluminum source flow;
step 2-2: performing thermal annealing treatment on the AlN layer based on first thermal annealing parameters, wherein the first thermal annealing parameters comprise a first thermal annealing temperature and a first thermal annealing time;
step 2-3: etching the AlN layer subjected to the thermal annealing treatment based on etching parameters, wherein the etching parameters comprise the proportion of boron trichloride and the proportion of chlorine gas flow, the third pressure of the reaction chamber, the power of the reaction chamber and the etching time;
step 2-4: and removing Ni metal on the surface of the etched AlN layer based on an acid solution corrosion process to obtain the AlN nano-pattern insertion layer.
9. The method of claim 6, wherein the step 9 comprises:
step 9-1: growing a p-type GaN layer on the p-type AlN layer based on GaN layer growth parameters, wherein the GaN layer growth parameters comprise a reaction chamber eighth temperature, a reaction chamber ninth pressure, a seventh ammonia gas flow, a third gallium source flow and a second magnesium source flow;
step 9-2: and carrying out thermal annealing treatment on the p-type GaN layer based on second thermal annealing parameters, wherein the second thermal annealing parameters comprise a second thermal annealing temperature and a second thermal annealing time length.
10. The method of claim 6, wherein the step 10 comprises:
based on the sputtering process, an n-type electrode is sputtered on the n-type AlN layer, and a p-type electrode is sputtered on the p-type GaN layer.
CN202110859939.3A 2021-07-28 2021-07-28 AlN ultraviolet light-emitting diode based on nano pattern insertion layer and preparation method thereof Active CN113764555B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110859939.3A CN113764555B (en) 2021-07-28 2021-07-28 AlN ultraviolet light-emitting diode based on nano pattern insertion layer and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110859939.3A CN113764555B (en) 2021-07-28 2021-07-28 AlN ultraviolet light-emitting diode based on nano pattern insertion layer and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113764555A true CN113764555A (en) 2021-12-07
CN113764555B CN113764555B (en) 2023-09-01

Family

ID=78788082

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110859939.3A Active CN113764555B (en) 2021-07-28 2021-07-28 AlN ultraviolet light-emitting diode based on nano pattern insertion layer and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113764555B (en)

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090072262A1 (en) * 2007-09-19 2009-03-19 The Regents Of The University Of California (Al,In,Ga,B)N DEVICE STRUCTURES ON A PATTERNED SUBSTRATE
CN102903810A (en) * 2011-07-27 2013-01-30 隆达电子股份有限公司 Light emitting diode and method for manufacturing the same
KR20130053974A (en) * 2011-11-16 2013-05-24 엘지이노텍 주식회사 Light emitting device
CN104269482A (en) * 2014-09-24 2015-01-07 杭州士兰明芯科技有限公司 LED substrate structure and manufacturing method of LED substrate structure
KR20150113525A (en) * 2014-03-31 2015-10-08 서울바이오시스 주식회사 Light emitting device having optical structure
CN105047775A (en) * 2015-05-29 2015-11-11 华灿光电股份有限公司 Ultraviolet light emitting diode epitaxial wafer and manufacturing method thereof
CN106848015A (en) * 2017-03-08 2017-06-13 王星河 A kind of nitride semiconductor LED and preparation method thereof
CN108091737A (en) * 2017-10-25 2018-05-29 华灿光电（浙江）有限公司 Light emitting diode chip and manufacturing method thereof
US20200176633A1 (en) * 2017-08-31 2020-06-04 Toshiba Materials Co., Ltd. Semiconductor light-emitting element and method for manufacturing same
TW202029529A (en) * 2019-01-25 2020-08-01 晶元光電股份有限公司 Light-emitting device and manufacturing method thereof

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090072262A1 (en) * 2007-09-19 2009-03-19 The Regents Of The University Of California (Al,In,Ga,B)N DEVICE STRUCTURES ON A PATTERNED SUBSTRATE
CN102903810A (en) * 2011-07-27 2013-01-30 隆达电子股份有限公司 Light emitting diode and method for manufacturing the same
KR20130053974A (en) * 2011-11-16 2013-05-24 엘지이노텍 주식회사 Light emitting device
KR20150113525A (en) * 2014-03-31 2015-10-08 서울바이오시스 주식회사 Light emitting device having optical structure
CN104269482A (en) * 2014-09-24 2015-01-07 杭州士兰明芯科技有限公司 LED substrate structure and manufacturing method of LED substrate structure
CN105047775A (en) * 2015-05-29 2015-11-11 华灿光电股份有限公司 Ultraviolet light emitting diode epitaxial wafer and manufacturing method thereof
CN106848015A (en) * 2017-03-08 2017-06-13 王星河 A kind of nitride semiconductor LED and preparation method thereof
US20200176633A1 (en) * 2017-08-31 2020-06-04 Toshiba Materials Co., Ltd. Semiconductor light-emitting element and method for manufacturing same
CN108091737A (en) * 2017-10-25 2018-05-29 华灿光电（浙江）有限公司 Light emitting diode chip and manufacturing method thereof
TW202029529A (en) * 2019-01-25 2020-08-01 晶元光電股份有限公司 Light-emitting device and manufacturing method thereof

Also Published As

Publication number Publication date
CN113764555B (en) 2023-09-01

Similar Documents

Publication Publication Date Title
JP4214585B2 (en) Semiconductor device, semiconductor device manufacturing method and manufacturing apparatus
KR100844722B1 (en) Growth method of nanocone and Fabricating method of light emitting diode using the same
US20070241352A1 (en) Group III Nitride Semiconductor Light Emitting Device
CN108899403B (en) Efficient light-emitting diode based on ScAlN/AlGaN superlattice p-type layer and preparation method
CN110224047B (en) Efficient light-emitting diode based on P-type doped AlScN/AlScN superlattice barrier layer and preparation method
JP2003023220A (en) Nitride semiconductor element
US10727054B2 (en) Nitride-based semiconductor device and method for preparing the same
US20060246614A1 (en) Method for manufacturing gallium nitride-based semiconductor device
CN103117346B (en) A kind of light-emitting diode chip for backlight unit and manufacture method thereof
CN107394022A (en) Efficient LED and preparation method based on nano thread structure
CN112885937B (en) Preparation method of P electrode of light-emitting diode chip with vertical structure
CN114864770A (en) Silicon-based gallium nitride epitaxial wafer and manufacturing method thereof
CN110518099A (en) A kind of efficient LED and production method
CN115064620A (en) Efficient deep ultraviolet light-emitting diode with YAlN/AlGaN superlattice p-type layer as step component and preparation method thereof
KR101852519B1 (en) Method for manufacturing optical element
CN112687773B (en) Epitaxial wafer of ultraviolet light-emitting diode and preparation method thereof
CN117577748A (en) LED epitaxial wafer, preparation method thereof and LED
JP2007095745A (en) Semiconductor light-emitting element and manufacturing method thereof, and luminaire using the same
CN113764555B (en) AlN ultraviolet light-emitting diode based on nano pattern insertion layer and preparation method thereof
CN109273568B (en) Gallium nitride-based light emitting diode epitaxial wafer and manufacturing method thereof
CN115347095B (en) Semiconductor device structure based on nitride single crystal substrate and application thereof
CN115863503A (en) Deep ultraviolet LED epitaxial wafer, preparation method thereof and deep ultraviolet LED
CN110148663A (en) A kind of LED epitaxial wafer and preparation method thereof
CN113013299B (en) Light emitting diode epitaxial wafer and growth method thereof
CN115274941A (en) Epitaxial wafer preparation method, epitaxial wafer and LED chip

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant