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CN106601878B - A kind of LED preparation method with high luminous efficiency - Google Patents

A kind of LED preparation method with high luminous efficiency Download PDF

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Publication number
CN106601878B
CN106601878B CN201611042592.9A CN201611042592A CN106601878B CN 106601878 B CN106601878 B CN 106601878B CN 201611042592 A CN201611042592 A CN 201611042592A CN 106601878 B CN106601878 B CN 106601878B
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CN106601878A (en
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梁沛明
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Guangdong Tianchengzhixing Lighting Technology Co ltd
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Guangdong Tiancheng Star Lighting Technology Co Ltd
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/01—Manufacture or treatment
    • H10H20/011—Manufacture or treatment of bodies, e.g. forming semiconductor layers
    • H10H20/013—Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials
    • H10H20/0137—Manufacture or treatment of bodies, e.g. forming semiconductor layers having light-emitting regions comprising only Group III-V materials the light-emitting regions comprising nitride materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/81—Bodies
    • H10H20/811—Bodies having quantum effect structures or superlattices, e.g. tunnel junctions
    • H10H20/812—Bodies having quantum effect structures or superlattices, e.g. tunnel junctions within the light-emitting regions, e.g. having quantum confinement structures
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/81—Bodies
    • H10H20/822—Materials of the light-emitting regions
    • H10H20/824—Materials of the light-emitting regions comprising only Group III-V materials, e.g. GaP
    • H10H20/825—Materials of the light-emitting regions comprising only Group III-V materials, e.g. GaP containing nitrogen, e.g. GaN
    • H10H20/8252—Materials of the light-emitting regions comprising only Group III-V materials, e.g. GaP containing nitrogen, e.g. GaN characterised by the dopants

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Led Devices (AREA)

Abstract

The LED preparation method with high photosynthetic efficiency that the invention discloses a kind of, this method can be further reduced light-emitting area loss, increase the growth quality that supplemental layers improve Quantum Well, improve backward voltage, while reducing device inside electric leakage, also utilize the oblique well layer of In content gradually variational, change the forbidden bandwidth of trap, to capture more electrons and holes, the contact area in electronics and hole is increased, light-emitting area is improved, reduces the speed of service of electronics, the effective electron number for increasing the contact with hole, improves the luminous efficiency of light emitting diode.

Description

A kind of LED preparation method with high photosynthetic efficiency
Technical field
The present invention relates to the preparation methods of LED, and in particular to a kind of LED preparation method with high photosynthetic efficiency.
Background technique
In recent years, it is known as light emitting diode (Light Emitting Diode, the LED) lighting engineering of " green illumination " Development is swift and violent.Compared with conventional illumination sources, white light emitting diode is not only low in energy consumption, and long service life, size is small, green ring It protects, has more the advantages that modulating performance is good, and response sensitivity is high.On the one hand white light emitting diode has transmission power high, right The features such as eye-safe；On the other hand, have that reaction speed is fast, modularity is good, no electromagnetic interference, without applying for radio-frequency spectrum The advantages that.
The chip that light emitting diode core is made of P-type semiconductor and N-type semiconductor, in P-type semiconductor and N-type There are a transition zone, referred to as PN junction between semiconductor.In the PN junction of certain semiconductor materials, the minority carrier of injection and more Extra energy is released can in the form of light when number Carrier recombination, so that electric energy is converted directly into luminous energy.
GaN base material belongs to direct band-gap semicondictor, and its band gap is continuously adjustable from 1.8~6.2V, is that production is highlighted Spend the most frequently used material of blue and green light and white light LEDs.However in the aluminium indium gallium nitrogen material of the direction c growth, there are very strong polarization Electric field, the electric field cause Quantum Well energy band to tilt, are spatially separated electrons and holes, reduce recombination luminescence efficiency.And And the barrier spike that energy band inclination generates can stop transporting for hole, hole effective mass is very big in addition, makes hole in each amount Distributed pole is uneven in sub- trap.
Light emitting diode is a kind of epitaxial structure generated by the way of epitaxial growth, and the epitaxial structure is mainly by serving as a contrast Bottom, provide electronics N-type layer, provide hole P-type layer and recombination region active layer composition, be mainly used in illumination, traffic The backlight of signal lamp, TV, mobile phone etc., blue, green, white light in backlight mainly use Metallo-Organic Chemical Vapor to deposit Method deposits to gallium nitride material to be formed in Sapphire Substrate.
In traditional gallium nitride based diode epitaxial slice structure, the dislocation through entire P~N knot is to cause diode One of the principal element that can be reduced, such dislocation will cause internal quantum efficiency reduction, reverse leakage, antistatic breakdown capability compared with Difference.
The Yanzhong outside LED electronic barrier layer PAlGaN cannot or lack, and main function is the high energy band using AlGaN Stop excessive to P layers of electronics of luminescent layer, but also brings many bad places.
Summary of the invention
The present invention provides a kind of LED preparation method with high photosynthetic efficiency, and this method can be further reduced light-emitting area damage It loses, increases the growth quality that supplemental layers improve Quantum Well, improve backward voltage, while reducing device inside electric leakage, also utilize The oblique well layer of In content gradually variational, changes the forbidden bandwidth of trap, to capture more electrons and holes, increases electronics and hole Contact area improves light-emitting area, reduces the speed of service of electronics, increases the effective electron number of the contact with hole, improves hair The luminous efficiency of optical diode.
To achieve the goals above, the present invention provides a kind of LED preparation method with high photosynthetic efficiency, which includes Following steps:
(1) preparing substrate
H2Environment high temperature purifies substrate；
(2) epitaxial wafer is formed on the substrate using Metal Organic Chemical Vapor Deposition method
The epitaxial wafer includes that low temperature buffer layer, U-shaped gallium nitride GaN layer, N-type are from bottom to top sequentially generated from substrate GaN layer, barrier layer/well layer/supplemental layers/oblique well layer structure multiple quantum well layer, functional layer, luminescent layer and p-type GaN layer；
(3) conductive layer is formed in p-type GaN layer
(4) etching N-GaN lateral wall forms N electrode, forms P electrode on the electrically conductive.
Preferably, in the step (1), in 1000 DEG C~1100 DEG C of H2Under atmosphere, it is passed through 100L/min~130L/ The H of min2, reaction cavity pressure 100mbar~300mbar is kept, substrate 8min~10min is handled.
Preferably, in the step (2), using Metal Organic Chemical Vapor Deposition method, at 550~580 DEG C, Reaction cavity pressure 300mbar~600mbar is kept, the NH that flow is 10000sccm~20000sccm is passed through3, 50sccm~ TMGa, 100L/min of 100sccm~130L/min H2, on substrate growth thickness be 20nm~40nm low temperature buffer layer GaN。
Preferably, in step (2), in the U-shaped GaN layer of low temperature buffer layer GaN growth:
2D type GaN layer is grown first, and growth temperature is 1050 DEG C, with a thickness of 0.05um, growth pressure 100torr；
Then fast cooling pressurization growth 3D type GaN layer, growth temperature are 990 DEG C, growth thickness 0.05um, growth pressure Power is 400torr.
Preferably, in the step (2), N-type GaN is the N-type GaN layer for adulterating Si, growth technique are as follows: keeps reaction It is cavity pressure, temperature-resistant, it is passed through the NH that flow is 30000sccm~60000sccm3, 200sccm~400sccm TMGa, The H of 100L/min~130L/min2, 20sccm~50sccm SiH4, the N-type GaN, Si of 3 μm~4 μm of continued propagation doping Si Doping concentration 5E18atoms/cm3~1E19atoms/cm3；Reaction cavity pressure, temperature-resistant is kept, being passed through flow is The NH of 30000sccm~60000sccm3, 300sccm~400sccm TMGa, 110L/min~130L/min H2、6sccm The SiH of~10sccm4, N-type GaN, the Si doping concentration 5E17atoms/cm of 300 μm~400 μm of continued propagation doping Si3~ 1E18atoms/cm3。
Preferably, in step (2), 10~15 periods are grown using Metal Organic Chemical Vapor Deposition method Barrier layer/well layer/supplemental layers/oblique well layer structure multiple quantum well layer:
A. in N2Or N2/H2Mixed atmosphere grows GaN barrier layer under the conditions of 850~870 DEG C；
B. in N2Or N2/H2Mixed atmosphere grows InGaN well layer under the conditions of 650~720 DEG C；
C. the growth of supplemental layers:
After well layer is grown, being passed through for the source metal Ga to be interrupted, continues to be passed through the source metal In, the break period is 10~25s, It is started to warm up simultaneously with the speed of 1.0~1.5 DEG C/s from the growth temperature of well layer, forms supplemental layers；
D. the growth of oblique well layer:
It is further continued for being passed through the source metal Ga, while continuing to heat up with the speed of 2.5~3 DEG C/s, form the oblique of In content gradually variational Well layer.
Preferably, in the step (2), the functional layer includes at least 3 circulation layers successively grown from the bottom to top, The circulation layer includes the N-type GaN layer for mixing element silicon successively grown from the bottom to top, mixes element silicon, aluminium element and phosphide element First AlInGaN layers of indium gallium nitride of N-type aluminium, AlInGaN layers of the second N-type of incorporation element silicon, aluminium element and phosphide element, and it is described AlInGaN layers of N-type GaN layer, first N-type for mixing element silicon are different with AlInGaN layers of second N-type of doping concentration.
Preferably, wherein the doping concentration of each layer of element silicon is 1e17/cm in the circulation layer3~1e19/cm3, mix The group of aluminium element is divided into 0.02wt%~0.5wt% in the miscellaneous layer for having aluminium element, doped with the group of phosphide element in the layer of phosphide element It is divided into 0.02wt%~0.05wt%.
Preferably, the growth temperature of above-mentioned functional layer be located at 750 DEG C~1000 DEG C within the scope of, pressure be located at 50torr~ Within the scope of 500torr, revolving speed be located at within the scope of 1000rpm~1500rpm, growth rate be located at 3 μm/h~5 μm/h range It is interior.
Preferably, in step (2), the luminescent layer is the In that alternating growth adulterates InxGa(1~x)N/GaN luminescent layer, Growth technique are as follows: keep reaction cavity pressure 400mbar~500mbar, 750 DEG C~800 DEG C of temperature, being passed through flow is The NH of 60000sccm~80000sccm3, 20sccm~40sccm TMGa, 1500sccm~2000sccm TMIn, 100L/ The N of min~130L/min2, the In of 2.5nm~3.5nm of growth doping InxGa(1~x)N layers, x=0.26~0.28, shine wave Long 450nm~455nm；Then temperature is increased to 750 DEG C~850 DEG C, is kept reaction cavity pressure 300mbar~400mbar, is passed through Flow is the NH of 50000sccm~70000sccm3, 20sccm~100sccm TMGa, 100L/min~130L/min N2, Grow the GaN layer of 8nm~15nm；Repeat InxGa(1~x)The growth of N, the then repeatedly growth of GaN, alternating growth InxGa(1~x) N/GaN luminescent layer, control periodicity are 10~12.
Preferably, in step (2), p-type GaN layer is generated in the following way: holding reaction cavity pressure 400mbar~ 950 DEG C~1000 DEG C of 900mbar, temperature are passed through the NH that flow is 50000sccm~70000sccm3, 20sccm~100sccm TMGa, 100L/min~130L/min H2, 1000sccm~3000sccm Cp2Mg, continued propagation 50nm~200nm's Mix the p-type GaN layer of Mg, Mg doping concentration 1E19atoms/cm3~1E20atoms/cm3。
Preferably, in the step (3), the conductive layer is metallic reflector.
The present invention has the advantage that light-emitting area loss can be further reduced, increases supplemental layers and improve Quantum Well Growth quality improves backward voltage, while reducing device inside electric leakage, also utilizes the oblique well layer of In content gradually variational, changes trap Forbidden bandwidth increase the contact area in electronics and hole to capture more electrons and holes, improve light-emitting area, drop The speed of service of low electronics increases the effective electron number of the contact with hole, improves the luminous efficiency of light emitting diode.
Specific embodiment
Embodiment one
H2Environment high temperature purifies substrate；In 1000 DEG C of H2Under atmosphere, it is passed through the H of 100L/min2, keep reaction chamber pressure Power 100mbar handles substrate 8min.
The epitaxial wafer includes that low temperature buffer layer, U-shaped gallium nitride GaN layer, N-type are from bottom to top sequentially generated from substrate GaN layer, barrier layer/well layer/supplemental layers/oblique well layer structure multiple quantum well layer, functional layer, luminescent layer and p-type GaN layer.
Using Metal Organic Chemical Vapor Deposition method, at 550 DEG C, reaction cavity pressure 300mbar is kept, stream is passed through Amount is the NH of 10000sccm3, 50sccm TMGa, 100L/min H2, on substrate growth thickness be 20nm low temperature buffer Layer GaN.
In the U-shaped GaN layer of low temperature buffer layer GaN growth: growth 2D type GaN layer first, growth temperature are 1050 DEG C, with a thickness of 0.05um, growth pressure 100torr；Then fast cooling pressurization growth 3D type GaN layer, growth temperature are 990 DEG C, growth thickness For 0.05um, growth pressure 400torr.
N-type GaN is the N-type GaN layer for adulterating Si, growth technique are as follows: keeps reaction cavity pressure, temperature-resistant, is passed through stream Amount is the NH of 30000sccm3, 200sccm TMGa, 100L/min~130L/min H2, 20sccm SiH4, continued propagation 3 μm doping Si N-type GaN, Si doping concentration 5E18atoms/cm3；Reaction cavity pressure, temperature-resistant is kept, being passed through flow is The NH of 30000sccm3, 300sccm TMGa, 110L/min H2, 6sccm SiH4, the N-type of 300 μm of continued propagation doping Si GaN, Si doping concentration 5E17atoms/cm3。
Barrier layer/well layer/supplemental layers/oblique the well layer in 10 periods is grown using Metal Organic Chemical Vapor Deposition method The multiple quantum well layer of structure: in N2Or N2/H2Mixed atmosphere grows GaN barrier layer under the conditions of 850 DEG C；In N2Or N2/H2Gaseous mixture Atmosphere grows InGaN well layer under the conditions of 650 DEG C；After well layer is grown, being passed through for the source metal Ga is interrupted, continues to be passed through metal In Source, break period 10s, while being started to warm up with the speed of 1.0 DEG C/s from the growth temperature of well layer, form supplemental layers；Followed by It is continuous to be passed through the source metal Ga, while continuing to heat up with the speed of 2.5/s, form the oblique well layer of In content gradually variational.
The functional layer includes at least 3 circulation layers successively grown from the bottom to top, and the circulation layer includes from the bottom to top The N-type GaN layer for mixing element silicon successively grown mixes the first N-type aluminium indium gallium nitride of element silicon, aluminium element and phosphide element AlInGaN layers, AlInGaN layers of the second N-type of incorporation element silicon, aluminium element and phosphide element, and the N-type GaN for mixing element silicon Layer, AlInGaN layer of first N-type and AlInGaN layers of second N-type of doping concentration difference.
Wherein the doping concentration of each layer of element silicon is 1e17/cm in the circulation layer3, doped in the layer of aluminium element The group of aluminium element is divided into 0.02wt%, is divided into 0.02wt% doped with the group of phosphide element in the layer of phosphide element.
The growth temperature of above-mentioned functional layer is located in 750 DEG C, pressure is located within the scope of 50torr, revolving speed is positioned at being Within the scope of 1000rpm, growth rate is located within the scope of 3 μm/h.
The luminescent layer is the In that alternating growth adulterates In0.26Ga0.74N/GaN luminescent layer, growth technique are as follows: keep anti- 750 DEG C of cavity pressure 400mbar, temperature are answered, the NH that flow is 60000sccm is passed through3, 20sccm TMGa, 1500sccm The N of TMIn, 100L/min2, the In of the 2.5nm of growth doping In0.26Ga0.74N layers, emission wavelength 450nm；Then temperature is increased To 750 DEG C, reaction cavity pressure 300mbar is kept, is passed through the NH that flow is 50000sccm3, 20sccm TMGa, 100L/min N2, grow the GaN layer of 8nm；Repeat In0.26Ga0.74The growth of N, the then repeatedly growth of GaN, alternating growth In0.26Ga0.74N/GaN luminescent layer, control periodicity are 10.
P-type GaN layer is generated in the following way: being kept reaction cavity pressure 400mbar~900mbar, 950 DEG C of temperature, is led to Inbound traffics are the NH of 50000sccm3, 20sccm TMGa, 100L/min~130L/min H2, 1000sccm Cp2Mg is held The p-type GaN layer for mixing Mg of continuous growth 50nm, Mg doping concentration 1E19atoms/cm3。
Conductive layer is formed in p-type GaN layer, the conductive layer is metallic reflector.It etches N-GaN lateral wall and forms N electricity Pole forms P electrode on the electrically conductive.
Embodiment two
H2Environment high temperature purifies substrate；In 1050 DEG C of H2Under atmosphere, it is passed through the H of 120L/min2, keep reaction chamber pressure Power 200mbar handles substrate 9min.
The epitaxial wafer includes that low temperature buffer layer, U-shaped gallium nitride GaN layer, N-type are from bottom to top sequentially generated from substrate GaN layer, barrier layer/well layer/supplemental layers/oblique well layer structure multiple quantum well layer, functional layer, luminescent layer and p-type GaN layer.
Using Metal Organic Chemical Vapor Deposition method, at 570 DEG C, reaction cavity pressure 450mbar is kept, stream is passed through Amount is the NH of 15000sccm3, 75sccm TMGa, 120L/min H2, on substrate growth thickness be 20nm~40nm it is low Warm buffer layer GaN.
In the U-shaped GaN layer of low temperature buffer layer GaN growth: growth 2D type GaN layer first, growth temperature are 1050 DEG C, with a thickness of 0.05um, growth pressure 100torr；Then fast cooling pressurization growth 3D type GaN layer, growth temperature are 990 DEG C, growth thickness For 0.05um, growth pressure 400torr.
N-type GaN is the N-type GaN layer for adulterating Si, growth technique are as follows: keeps reaction cavity pressure, temperature-resistant, is passed through stream Amount is the NH of 45000sccm3, 300sccm TMGa, 120L/min H2, 40sccm SiH4, 3.5 μm of doping Si of continued propagation N-type GaN, Si doping concentration 7.5E18atoms/cm3；Reaction cavity pressure, temperature-resistant is kept, being passed through flow is The NH of 40000sccm3, 350sccm TMGa, 120L/min H2, 8sccm SiH4, the N-type of 350 μm of continued propagation doping Si GaN, Si doping concentration 7.5E17atoms/cm3。
Barrier layer/well layer/supplemental layers/oblique the well layer in 12 periods is grown using Metal Organic Chemical Vapor Deposition method The multiple quantum well layer of structure: in N2Or N2/H2Mixed atmosphere grows GaN barrier layer under the conditions of 860 DEG C；In N2Or N2/H2Gaseous mixture Atmosphere grows InGaN well layer under the conditions of 700 DEG C；After well layer is grown, being passed through for the source metal Ga is interrupted, continues to be passed through metal In Source, break period 15s, while being started to warm up with the speed of 1.3 DEG C/s from the growth temperature of well layer, form supplemental layers；Followed by It is continuous to be passed through the source metal Ga, while continuing to heat up with the speed of 2.7 DEG C/s, form the oblique well layer of In content gradually variational.
The functional layer includes at least 3 circulation layers successively grown from the bottom to top, and the circulation layer includes from the bottom to top The N-type GaN layer for mixing element silicon successively grown mixes the first N-type aluminium indium gallium nitride of element silicon, aluminium element and phosphide element AlInGaN layers, AlInGaN layers of the second N-type of incorporation element silicon, aluminium element and phosphide element, and the N-type GaN for mixing element silicon Layer, AlInGaN layer of first N-type and AlInGaN layers of second N-type of doping concentration difference.
Wherein the doping concentration of each layer of element silicon is 1e18/cm in the circulation layer3, doped in the layer of aluminium element The group of aluminium element is divided into 0.4wt%, is divided into 0.03wt% doped with the group of phosphide element in the layer of phosphide element.
The growth temperature of above-mentioned functional layer is located in 800 DEG C, pressure is located within the scope of 200torr, revolving speed is positioned at being Within the scope of 1200rpm, growth rate is located within the scope of 4 μm/h.
The luminescent layer is the In that alternating growth adulterates In0.27Ga0.73N/GaN luminescent layer, growth technique are as follows: keep anti- 775 DEG C of cavity pressure 450mbar, temperature are answered, the NH that flow is 70000sccm is passed through3, 30sccm TMGa, 1700sccm TMIn, 100L/min~130L/min N2, the In of the 3nm of growth doping In0.27Ga0.73N layers, emission wavelength 453nm；Then Temperature is increased to 800 DEG C, keeps reaction cavity pressure 360mbar, is passed through the NH that flow is 60000sccm3, 70sccm TMGa, The N of 12L/min2, grow the GaN layer of 10nm；Repeat In0.27Ga0.73The growth of N, the then repeatedly growth of GaN, alternating growth In0.27Ga0.73N/GaN luminescent layer, control periodicity are 11.
P-type GaN layer is generated in the following way: keeping reaction cavity pressure 600mbar, 975 DEG C of temperature, being passed through flow is The NH of 60000sccm3, 50sccm TMGa, 120L/min H2, 2000sccm Cp2Mg, continued propagation 100nm's mixes Mg's P-type GaN layer, Mg doping concentration 1E19atoms/cm3~1E20atoms/cm3。
Conductive layer is formed in p-type GaN layer, the conductive layer is metallic reflector.It etches N-GaN lateral wall and forms N electricity Pole forms P electrode on the electrically conductive.
Embodiment three
H2Environment high temperature purifies substrate；In 1100 DEG C of H2Under atmosphere, it is passed through the H of 130L/min2, keep reaction chamber pressure Power 300mbar handles substrate 10min.
The epitaxial wafer includes that low temperature buffer layer, U-shaped gallium nitride GaN layer, N-type are from bottom to top sequentially generated from substrate GaN layer, barrier layer/well layer/supplemental layers/oblique well layer structure multiple quantum well layer, functional layer, luminescent layer and p-type GaN layer.
Using Metal Organic Chemical Vapor Deposition method, at 580 DEG C, reaction cavity pressure 600mbar is kept, stream is passed through Amount is the NH of 20000sccm3, 100sccm TMGa, 130L/min H2, on substrate growth thickness be 40nm low temperature buffer Layer GaN.
In the U-shaped GaN layer of low temperature buffer layer GaN growth: growth 2D type GaN layer first, growth temperature are 1050 DEG C, with a thickness of 0.05um, growth pressure 100torr；Then fast cooling pressurization growth 3D type GaN layer, growth temperature are 990 DEG C, growth thickness For 0.05um, growth pressure 400torr.
N-type GaN is the N-type GaN layer for adulterating Si, growth technique are as follows: keeps reaction cavity pressure, temperature-resistant, is passed through stream Amount is the NH of 60000sccm3, 400sccm TMGa, 130L/min H2, 50sccm SiH4, 4 μm of continued propagation are adulterated Si's N-type GaN, Si doping concentration 1E19atoms/cm3；Reaction cavity pressure, temperature-resistant is kept, being passed through flow is 60000sccm's NH3, 400sccm TMGa, 130L/min H2, 6sccm~10sccm SiH4, the N-type of 400 μm of continued propagation doping Si GaN, Si doping concentration 1E18atoms/cm3。
Using Metal Organic Chemical Vapor Deposition method grow 10~15 periods barrier layer/well layer/supplemental layers/tiltedly The multiple quantum well layer of well layer structure: in N2Or N2/H2Mixed atmosphere grows GaN barrier layer under the conditions of 870 DEG C；In N2Or N2/H2 is mixedIt closes Atmosphere grows InGaN well layer under the conditions of 720 DEG C；After well layer is grown, being passed through for the source metal Ga is interrupted, continues to be passed through metal The source In, break period 25s, while being started to warm up with the speed of 1.5 DEG C/s from the growth temperature of well layer, form supplemental layers；Again Continue to be passed through the source metal Ga, while continuing to heat up with the speed of 3 DEG C/s, forms the oblique well layer of In content gradually variational.
The functional layer includes at least 3 circulation layers successively grown from the bottom to top, and the circulation layer includes from the bottom to top The N-type GaN layer for mixing element silicon successively grown mixes the first N-type aluminium indium gallium nitride of element silicon, aluminium element and phosphide element AlInGaN layers, AlInGaN layers of the second N-type of incorporation element silicon, aluminium element and phosphide element, and the N-type GaN for mixing element silicon Layer, AlInGaN layer of first N-type and AlInGaN layers of second N-type of doping concentration difference.
Wherein the doping concentration of each layer of element silicon is 1e19/cm in the circulation layer3, doped in the layer of aluminium element The group of aluminium element is divided into 0.5wt%, is divided into 0.05wt% doped with the group of phosphide element in the layer of phosphide element.
The growth temperature of above-mentioned functional layer is located in 1000 DEG C, pressure is located within the scope of 500torr, revolving speed is positioned at being Within the scope of 1500rpm, growth rate is located within the scope of 5 μm/h.
The luminescent layer is the In that alternating growth adulterates In0.28Ga0.72N/GaN luminescent layer, growth technique are as follows: keep anti- 800 DEG C of cavity pressure 500mbar, temperature are answered, the NH that flow is 80000sccm is passed through3, 40sccm TMGa, 2000sccm The N of TMIn, 130L/min2, the In of 2.5nm~3.5nm of growth doping In0.28Ga0.72N layers of emission wavelength 455nm；Then it rises High-temperature keeps reaction cavity pressure 300mbar~400mbar to 850 DEG C, is passed through the NH that flow is 70000sccm3、100sccm TMGa, 130L/min N2, grow the GaN layer of 15nm；Repeat In0.28Ga0.72The growth of N, the then repeatedly growth of GaN are handed over For growth In0.28Ga0.72N/GaN luminescent layer, control periodicity are 12.
P-type GaN layer is generated in the following way: keeping reaction cavity pressure 900mbar, 1000 DEG C of temperature, being passed through flow is The NH of 70000sccm3, 100sccm TMGa, 130L/min H2, 1000sccm~3000sccm Cp2Mg, continued propagation The p-type GaN layer for mixing Mg of 50nm~200nm, Mg doping concentration 1E20atoms/cm3。
Conductive layer is formed in p-type GaN layer, the conductive layer is metallic reflector.It etches N-GaN lateral wall and forms N electricity Pole forms P electrode on the electrically conductive.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist Under the premise of not departing from present inventive concept, several equivalent substitute or obvious modifications is made, and performance or use is identical, all should It is considered as belonging to protection scope of the present invention.

Claims (8)

1.一种具有高光效的LED制备方法，该制备方法包括如下步骤：1. A LED preparation method with high luminous efficiency, the preparation method comprising the steps: （1）准备衬底(1) Prepare the substrate H2环境中高温净化衬底；High temperature purification of substrates in H2 environment; （2）采用金属有机化合物化学气相沉积法在衬底上形成外延片(2) Forming epitaxial wafers on substrates by metal organic compound chemical vapor deposition 所述外延片包括从衬底上由下而上依次生成低温缓冲层、U型氮化镓GaN层、N型GaN层、垒层/阱层/补充层/斜阱层结构的多量子阱层、功能层、发光层和P型GaN层；The epitaxial wafer includes a multi-quantum well layer in which a low-temperature buffer layer, a U-type gallium nitride GaN layer, an N-type GaN layer, a barrier layer/well layer/supplementary layer/inclined well layer structure are sequentially formed from the substrate from bottom to top , functional layer, light-emitting layer and P-type GaN layer; （3）在P型GaN层上形成导电层；(3) forming a conductive layer on the P-type GaN layer; （4）蚀刻N-GaN外侧壁形成N电极，在导电层上形成P电极；(4) Etch the outer sidewall of N-GaN to form an N electrode, and form a P electrode on the conductive layer; 在步骤（2）中，采用金属有机化合物化学气相沉积法生长10~15个周期的垒层/阱层/补充层/斜阱层结构的多量子阱层：In step (2), a multi-quantum well layer with a barrier layer/well layer/supplementary layer/inclined well layer structure of 10 to 15 periods is grown by metal organic compound chemical vapor deposition method: a. 在N2或N2/H2混合气氛、850~870℃条件下生长GaN垒层；a. Grow the GaN barrier layer in a mixed atmosphere of N 2 or N 2 /H 2 at 850~870℃; b. 在N2或N2/H2混合气氛、650~720℃条件下生长InGaN阱层；b. Grow the InGaN well layer in a mixed atmosphere of N 2 or N 2 /H 2 at 650~720°C; c. 补充层的生长：c. Growth of the complementary layer: 阱层生长结束后，中断金属Ga源的通入，继续通入金属In源，中断时间为10～25s，同时以1.0～1.5℃/s的速度从阱层的生长温度开始升温，形成补充层；After the growth of the well layer is completed, the supply of the metal Ga source is interrupted, and the metal In source is continued to be supplied for 10 to 25 s. At the same time, the temperature rises from the growth temperature of the well layer at a rate of 1.0 to 1.5 °C/s to form a supplementary layer. ; d．斜阱层的生长：d. Growth of inclined well layers: 再继续通入金属Ga源，同时以2.5~3℃/s的速度继续升温，形成In组分渐变的斜阱层；Continue to pass in the metal Ga source, and at the same time continue to heat up at a rate of 2.5~3°C/s to form an inclined well layer with graded In composition; 在所述步骤（2）中，所述功能层至少包括3个由下至上依次生长的循环层，所述循环层包括由下至上依次生长的掺硅元素的N型GaN层，掺硅元素、铝元素和铟元素的第一N型铝铟氮化镓AlInGaN层，掺入硅元素、 铝元素和铟元素的第二N型AlInGaN层，且所述掺硅元素的N型GaN层、所述第一N型AlInGaN层和所述第二N型AlInGaN层的掺杂浓度不同。In the step (2), the functional layer includes at least three circulating layers that grow sequentially from bottom to top, the circulating layers include N-type GaN layers doped with silicon elements that grow sequentially from bottom to top, silicon-doped elements, A first N-type AlInGaN AlInGaN layer with aluminum and indium elements, a second N-type AlInGaN layer doped with silicon, aluminum, and indium elements, and the silicon-doped N-type GaN layer, the The doping concentrations of the first N-type AlInGaN layer and the second N-type AlInGaN layer are different. 2.如权利要求1所述的方法，其特征在于，在所述步骤（1）中，在1000℃~1100℃的H2气氛下，通入100L/min~130L/min的H2，保持反应腔压力100mbar~300mbar，处理衬底8min~10min。2 . The method according to claim 1 , wherein, in the step (1), under the H 2 atmosphere of 1000° C. to 1100° C., the H 2 of 100 L/min to 130 L/min is fed, and the The pressure of the reaction chamber is 100mbar~300mbar, and the substrate is processed for 8min~10min. 3.如权利要求2所述的方法，其特征在于，在所述步骤（2）中，采用金属有机化合物化学气相沉积法，在550~580℃，保持反应腔压力300mbar~600mbar，通入流量为10000sccm~20000sccm的NH3、50sccm~100sccm的TMGa、100L/min~130L/min的H2、在衬底上生长厚度为20nm~40nm的低温缓冲层GaN。3. The method according to claim 2, characterized in that, in the step (2), a metal-organic compound chemical vapor deposition method is used, at 550-580° C., the reaction chamber pressure is maintained at 300mbar-600mbar, and the flow rate is 10000sccm~20000sccm NH 3 , 50sccm~100sccm TMGa, 100L/min~130L/min H 2 , and a low temperature buffer layer GaN with a thickness of 20nm~40nm is grown on the substrate. 4.如权利要求3所述的方法，其特征在于，在步骤（2）中，在低温缓冲层GaN生长U型GaN层：4. The method of claim 3, wherein in step (2), a U-type GaN layer is grown on the low temperature buffer layer GaN: 首先生长2D型GaN层，生长温度为1050℃，厚度为0.05um，生长压力100torr；First, grow a 2D GaN layer with a growth temperature of 1050°C, a thickness of 0.05um, and a growth pressure of 100torr; 然后快速降温增压生长3D型GaN层，生长温度为990℃，生长厚度为0.05um,生长压力为400torr。Then, the 3D-type GaN layer is grown by rapid cooling and pressurization. The growth temperature is 990°C, the growth thickness is 0.05um, and the growth pressure is 400torr. 5.如权利要求4所述的方法，其特征在于，在所述步骤（2）中，N型GaN为掺杂Si的N型GaN层，其生长工艺为：保持反应腔压力、温度不变，通入流量为30000sccm~60000sccm的NH3、200sccm~400sccm的TMGa、100L/min~130L/min的H2、20sccm~50sccm的SiH4，持续生长3μm~4μm掺杂Si的N型GaN，Si掺杂浓度5E18atoms/cm3~1E19atoms/cm3；保持反应腔压力、温度不变，通入流量为30000sccm~60000sccm的NH3、300sccm~400sccm的TMGa、110L/min~130L/min的H2、6sccm~10sccm的SiH4，持续生长300μm~400μm掺杂Si的N型GaN，Si掺杂浓度5E17atoms/cm3~1E18atoms/cm3。5 . The method according to claim 4 , wherein in the step (2), the N-type GaN is an N-type GaN layer doped with Si, and the growth process is: keeping the pressure and temperature of the reaction chamber unchanged. 6 . , the flow rate is 30000sccm~60000sccm NH 3 , 200sccm~400sccm TMGa, 100L/min~130L/min H 2 , 20sccm~50sccm SiH 4 , continue to grow 3μm~4μm Si-doped N-type GaN, Si The doping concentration is 5E18atoms/cm 3 ~1E19 atoms/cm 3 ; keep the pressure and temperature of the reaction chamber unchanged, and the flow rate is 30000sccm~60000sccm NH 3 , 300sccm~400sccm TMGa, 110L/min~130L/min H 2 , SiH 4 of 6sccm~10sccm, continuous growth of 300μm~400μm Si-doped N-type GaN, Si doping concentration is 5E17atoms/ cm3 ~1E18atoms/ cm3 . 6.如权利要求5所述的方法，其特征在于，在步骤（2）中，所述发光层为交替生长掺杂In的InxGa(1~x)N/GaN发光层，其生长工艺为：保持反应腔压力400mbar~500mbar、温度750℃~800℃，通入流量为60000sccm~80000sccm的NH3、20sccm~40sccm的TMGa、1500sccm~2000sccm的TMIn、100L/min~130L/min的N2，生长掺杂In的2.5nm~3.5nm的InxGa(1~x)N层，x＝0.26~0.28，发光波长450nm~455nm；接着升高温度至750℃~850℃，保持反应腔压力300mbar~400mbar，通入流量为50000sccm~70000sccm的NH3、20sccm~100sccm的TMGa、100L/min~130L/min的N2，生长8nm~15nm的GaN层；重复InxGa(1~x)N的生长，然后重复GaN的生长，交替生长InxGa (1~x)N/GaN发光层，控制周期数为10~12个。6 . The method of claim 5 , wherein in step (2), the light-emitting layer is an alternately grown InxGa (1~x) N /GaN light-emitting layer doped with In, and the growth process thereof is the method of claim 5 . To keep the pressure of the reaction chamber at 400mbar~500mbar, the temperature at 750℃~800℃, and the flow rate of NH 3 of 60000sccm~80000sccm, TMGa of 20sccm~40sccm, TMIn of 1500sccm~2000sccm, and N2 of 100L/min~130L/min , grow In x Ga (1~x) N layer doped with In 2.5nm~3.5nm, x=0.26~0.28, light emission wavelength 450nm~455nm; then raise the temperature to 750℃~850℃, keep the pressure of the reaction chamber 300mbar~400mbar, the flow rate is 50000sccm~70000sccm NH3 , 20sccm~100sccm TMGa, 100L/min~130L/min N2 , grow 8nm~15nm GaN layer; repeat In x Ga (1~x) N The growth of GaN is repeated, and the In x Ga (1~x) N/GaN light-emitting layer is grown alternately, and the number of controlled cycles is 10~12. 7.如权利要求6所述的方法，其特征在于，在步骤（2）中，采用如下方式生成P型GaN层：保持反应腔压力400mbar~900mbar、温度950℃~1000℃，通入流量为50000sccm~70000sccm的NH3、20sccm~100sccm的TMGa、100L/min~130L/min的H2、1000sccm~3000sccm的Cp2Mg，持续生长50nm~200nm的掺Mg的P型GaN层，Mg掺杂浓度1E19atoms/cm3~1E20atoms/cm3。7. The method according to claim 6, characterized in that, in step (2), the P-type GaN layer is generated in the following manner: maintaining the pressure of the reaction chamber at 400mbar~900mbar, the temperature at 950℃~1000℃, and the flow rate of 50000sccm~70000sccm NH 3 , 20sccm~100sccm TMGa, 100L/min~130L/min H 2 , 1000sccm~3000sccm Cp 2 Mg, continue to grow 50nm~200nm Mg-doped P-type GaN layer, Mg doping concentration 1E19atoms/cm 3 ~1E20atoms/cm 3 . 8.如权利要求7所述的方法，其特征在于，在所述步骤（3）中，所述导电层为金属反射层。8 . The method of claim 7 , wherein, in the step (3), the conductive layer is a metal reflective layer. 9 .
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