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CN103811601B - A kind of GaN base LED multi-level buffer layer growth method with Sapphire Substrate as substrate - Google Patents

A kind of GaN base LED multi-level buffer layer growth method with Sapphire Substrate as substrate Download PDF

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CN103811601B
CN103811601B CN201410090745.1A CN201410090745A CN103811601B CN 103811601 B CN103811601 B CN 103811601B CN 201410090745 A CN201410090745 A CN 201410090745A CN 103811601 B CN103811601 B CN 103811601B
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何成中
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Ningbo anxinmei Semiconductor Co.,Ltd.
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Hefei Irico Epilight Technology Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor 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
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    • H01L33/0062Processes for devices with an active region comprising only III-V compounds
    • H01L33/0066Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
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    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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    • HELECTRICITY
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    • H01L33/00Semiconductor 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
    • H01L33/02Semiconductor 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
    • H01L33/04Semiconductor 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 quantum effect structure or superlattice, e.g. tunnel junction
    • H01L33/06Semiconductor 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 quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier

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Abstract

The present invention provides a kind of GaN base LED multi-level buffer layer growth method with Sapphire Substrate as substrate, its multi-level buffer layer epitaxial structure, the growing method of its epitaxial structure includes step in detail below: substrate carries out in hydrogen atmosphere high-temperature cleaning process, 600 DEG C are dropped at a temperature of Jiang, adjust epitaxial growth atmosphere to prepare to grow multistage LT-AlGaN/MT-GaN/HT-GaN cushion, growth GaN non-doped layer afterwards, the N-type GaN layer that growth doping content is stable, grow shallow quantum well layer, growth luminescent layer multiple quantum well layer, growing low temperature p-type GaN layer, growth PAlGaN current barrier layer, high temperature p-type GaN layer, p-type contact layer, epitaxial growth uses pure nitrogen gas atmosphere to make annealing treatment after terminating.The present invention preferably solves the Macrolattice mismatch problem between sapphire and GaN by multistage LT-AlGaN/MT-GaN/HT-GaN buffer layer structure, reduces threading dislocation, improves crystal mass, reduces electric leakage and improves the brightness of epitaxial wafer, improves LED luminous efficiency.

Description

A kind of GaN base LED multi-level buffer layer growth method with Sapphire Substrate as substrate
Technical field
The present invention relates to GaN base light emitting diode (LED) technical field of material, be specially a kind of with blue precious It it is the GaN base LED multi-level buffer layer growth method of substrate at the bottom of stone lining.
Background technology
Volume is little, energy because it has for semiconductor light-emitting-diode (light-emission diodes, LED) Consume low, life-span length, the advantage such as environmental and durable, obtain very in fields such as display lamp, display screen, backlights Good application.At present blue, green light LED mainly use GaN as matrix material, because GaN is the width of direct band gap Bandgap semiconductor material, its ternary alloy three-partalloy InxGa1-xThe energy band band gap of N (x=0~1) can be from 0.7eV(InN) To 3.4eV(GaN) continuously adjustabe, emission wavelength covering visible light and the whole region of black light.Recently Along with LED is in the extensive application in white-light illuminating field, the LED of high brightness becomes the main target that people pursue.
In the epitaxial layer of gallium nitride-based light-emitting diode growth course grown with sapphire for substrate, due to blue precious There is significant lattice mismatch in stone and GaN, GaN base light LED material can produce the biggest in growth course Stress.This stress influences whether the internal quantum efficiency of epitaxial wafer and the brightness of epitaxial wafer, the most also can affect To antistatic effect, in typical epitaxial layer structure, with low-temperature gan layer as cushion, this layer is in epitaxial growth In have great role.And for cushion, the effect that different growing methods is played varies in size, the heaviest Stress in the effect wanted such as release crystallization process, blocks up the threading dislocation that goes out, improves crystal mass etc..
Summary of the invention
Technical problem solved by the invention is to provide a kind of GaN base LED with Sapphire Substrate as substrate Multi-level buffer layer growth method, to solve the problem in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions: one with Sapphire Substrate is The GaN base LED multi-level buffer layer growth method of substrate, its multi-level buffer layer epitaxial structure, from bottom to top suitable Sequence includes successively: substrate, multistage LT-AlGaN/MT-GaN/HT-GaN cushion, GaN non-doped layer, N Type GaN layer, shallow quantum well layer, luminescent quantum well layer, low temperature p-type GaN layer, PAlGaN current barrier layer, High temperature p-type GaN layer, p-type contact layer, the growing method of its epitaxial structure includes step in detail below:
(1) substrate is carried out in 1000-1200 DEG C of hydrogen atmosphere high-temperature cleaning and processes 5-20min, then Carrying out nitrogen treatment, substrate is sapphire material;
(2) drop to 600 DEG C at a temperature of inciting somebody to action, adjust the preparation growth of epitaxial growth atmosphere multistage LT-AlGaN/MT-GaN/HT-GaN cushion, described multistage LT-AlGaN/MT-GaN/HT-GaN cushion bag Include multiple LT-AlGaN/MT-GaN/HT-GaN structure overlapping successively, at high temperature through H2Processed is blue precious Stone grown on substrates AlGaN layer is 600 DEG C, epitaxial growth under the conditions of reaction cavity pressure 500Torr, thick Degree is 10-30nm;After AlGaN layer has grown, temperature is increased to 1010-1100 DEG C and carries out at thermal annealing Reason;Afterwards, MT-GaN layer 950 DEG C, under the conditions of reaction cavity pressure 400Torr with 4.0-10.0 μm/h High development speed carries out epitaxial growth, and thickness is 0.2-2 μm;HT-GaN layer temperature be 1080 degree, anti- Carrying out epitaxial growth with 2.0-4.0 μm/low growth rate of h under the conditions of answering chamber pressure 200Torr, thickness is 0.1-2 μm, finally through H under the conditions of 1000-1010 DEG C2Gas disposal epitaxial surface, prepares growth next week Phase, multistage LT-AlGaN/MT-GaN/HT-GaN buffer layer structure 2-20 the cycle of overlapping growth successively;
(3), after described multistage LT-AlGaN/MT-GaN/HT-GaN buffer growth terminates, temperature is regulated To 1000-1200 DEG C, epitaxial growth thickness is the GaN non-doped layer of 0.5-2 μm, and growth pressure is 100-300Torr, V/III ratio is 100-3000;
(4) after the growth of described GaN non-doped layer terminates, the N-type GaN layer that growth doping content is stable is thick Degree is 2.4-8.4 μm, and growth temperature is 1000-1200 DEG C, and pressure is 100-600Torr, and V/III ratio is 100-3000;
(5) after the growth of described N-type GaN layer terminates, growing shallow quantum well layer, described shallow quantum well layer includes 3-15 quantum well structure overlapping successively, growth temperature is 820-920 DEG C, and growth pressure is 100-500Torr, V/III ratio is 300-5000, and thickness is 10-200nm;
(6) after the growth of described shallow quantum well layer terminates, growing luminescent layer multiple quantum well layer, growth temperature is 700-850 DEG C, growth pressure is 100-500Torr, and V/III mol ratio is 300-5000, described luminescence Layer MQW is by the In in 6-12 cycleyGa1-yN (x < y < 1)/GaN MQW composition, described InyGa1-yN (x < y < 1) quantum well layer thickness is 2-5nm, and growth temperature is 720-820 DEG C;Described GaN barrier layer Thickness is 8-15nm, and growth temperature is 820-920 DEG C, and growth pressure is 100-500Torr, and V/III rubs That ratio is 300-5000;
(7), after the growth of described luminescent layer quantum well layer terminates, growth thickness is the low temperature p-type of 10-100nm GaN layer, growth temperature is 620-820 DEG C, and growth time is 5-35min, and growth pressure is 100-500Torr, V/III ratio is 300-5000;
(8), after the growth of described low temperature p-type GaN layer terminates, growth thickness is the PAlGaN electricity of 10-200nm Flow barrier, growth temperature is 800-1200 DEG C, and growth time is 2-18min, and growth pressure is 50-500Torr, V/III than be 10-1000, in p-type AlGaN layer the molar constituent content of Al be 5%~ 30%;
(9), after the growth of described PAlGaN current barrier layer terminates, growth thickness is the high temperature P of 100-800nm Type GaN layer, growth temperature is 850-950 DEG C, and growth time is 5-40min, and growth pressure is 100-500Torr, V/III ratio is 300-5000;
(10), after the growth of described high temperature p-type GaN layer terminates, growth thickness is the p-type contact layer of 5-20nm, Growth temperature is 850-1050 DEG C, and growth time is 1-10min, and growth pressure is 100-500Torr, V/ III ratio is 1000-20000;
(11) after epitaxial growth terminates, the temperature of reative cell is down to 650-800 DEG C, uses pure nitrogen gas atmosphere Carry out making annealing treatment 2-15min, be then down to room temperature, subsequently, after over cleaning, deposition, photoetching and etching Continuous processing technique makes single small-size chips.
With trimethyl gallium (TMGa), triethyl-gallium (TEGa), trimethyl in the growth course of described epitaxial structure Aluminum (TMAl), trimethyl indium (TMIn) and ammonia (NH3) respectively as Ga, Al, In and N source.
With silane (SiH in the growth course of described epitaxial structure4) and two cyclopentadienyl magnesium (CP2Mg) respectively as N, P-type dopant.
With hydrogen (H in the growth course of described epitaxial structure2) or nitrogen (N2) as carrier gas.
Compared with disclosed technology, there is advantages below in the present invention: the present invention is by multistage LT-AlGaN/MT-GaN/HT-GaN buffer layer structure preferably solves the big lattice between sapphire and GaN and loses Join problem, the stress between sapphire and GaN can be reduced, reduce threading dislocation, improve crystal mass, subtract Little electric leakage;Meanwhile, this kind of growing method can periodically progressively bury in oblivion during alternating growth from substrate with The threading dislocation that GaN interface produces, reduces threading dislocation further, thus reduces the non-radiative multiple of active area Conjunction center, improves the brightness of epitaxial wafer, improves LED luminous efficiency.
Accompanying drawing explanation
Fig. 1 is the epitaxial layer multistage LT-AlGaN/MT-GaN/HT-GaN buffer layer structure growth signal of the present invention Figure.
Detailed description of the invention
In order to make the technological means of the present invention, creation characteristic, workflow, using method reach purpose and merit Effect is easy to understand, and below in conjunction with the embodiment of the present invention, enters the technical scheme in the embodiment of the present invention Row clearly and completely describes, it is clear that described embodiment is only a part of embodiment of the present invention, and It is not all, of embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art are not making The every other embodiment obtained under creative work premise, broadly falls into the scope of protection of the invention.
Embodiment 1
A kind of GaN base LED multi-level buffer layer growth method with Sapphire Substrate as substrate, its multi-level buffer layer Epitaxial structure, order from bottom to top includes successively: substrate, multistage LT-AlGaN/MT-GaN/HT-GaN are slow Rush layer, GaN non-doped layer, N-type GaN layer, shallow quantum well layer, luminescent quantum well layer, low temperature p-type GaN Layer, PAlGaN current barrier layer, high temperature p-type GaN layer, p-type contact layer, the growing method of its epitaxial structure Including step in detail below:
(1) substrate is carried out in 1000 DEG C of hydrogen atmospheres high-temperature cleaning and processes 5min, then nitrogenize Processing, substrate is sapphire material;
(2) drop to 600 DEG C at a temperature of inciting somebody to action, adjust the preparation growth of epitaxial growth atmosphere multistage LT-AlGaN/MT-GaN/HT-GaN cushion, described multistage LT-AlGaN/MT-GaN/HT-GaN cushion bag Include multiple LT-AlGaN/MT-GaN/HT-GaN structure overlapping successively, at high temperature through H2Processed is blue precious Stone grown on substrates AlGaN layer is 600 DEG C, epitaxial growth under the conditions of reaction cavity pressure 500Torr, thick Degree is 10-30nm;After AlGaN layer has grown, temperature is increased to 1010-1100 DEG C and carries out at thermal annealing Reason;Afterwards, MT-GaN layer 950 DEG C, become with 4.0 μm/h height under the conditions of reaction cavity pressure 400Torr Long speed carries out epitaxial growth, and thickness is 0.2 μm;HT-GaN layer is 1080 DEG C, reaction cavity pressure in temperature Carrying out epitaxial growth with the low growth rate of 2.0 μm/h under the conditions of power 200Torr, thickness is 0.1 μm, finally Through H under the conditions of 1000 DEG C2Gas disposal epitaxial surface, prepares growth next cycle, multistage LT-AlGaN/MT-GaN/HT-GaN buffer layer structure 2 cycles of overlapping growth successively;
(3), after described multistage LT-AlGaN/MT-GaN/HT-GaN buffer growth terminates, temperature is regulated To 1000 DEG C, epitaxial growth thickness is the GaN non-doped layer of 0.5 μm, and growth pressure is 100Torr, V / III ratio is 100;
(4) after the growth of described GaN non-doped layer terminates, the N-type GaN layer that growth doping content is stable is thick Degree is 2.4 μm, and growth temperature is 1000 DEG C, and pressure is 100Torr, and V/III ratio is 100;
(5) after the growth of described N-type GaN layer terminates, growing shallow quantum well layer, described shallow quantum well layer includes 3 quantum well structures overlapping successively, growth temperature is 820 DEG C, and growth pressure is 100Torr, V/III ratio Being 300, thickness is 10nm;
(6) after the growth of described shallow quantum well layer terminates, growing luminescent layer multiple quantum well layer, growth temperature is 700 DEG C, growth pressure is 100Torr, and V/III mol ratio is 300, and described luminescent layer MQW is by 6 The In in individual cycleyGa1-yN (x < y < 1)/GaN MQW composition, described InyGa1-yN (x < y < 1) quantum well layer Thickness is 2nm, and growth temperature is 720 DEG C;Described GaN barrier layer thickness is 8nm, and growth temperature is 820 DEG C, Growth pressure is 100Torr, and V/III mol ratio is 300;
(7), after the growth of described luminescent layer quantum well layer terminates, growth thickness is low temperature p-type GaN of 10nm Layer, growth temperature is 620 DEG C, and growth time is 5min, and growth pressure is 100Torr, and V/III ratio is 300;
(8), after the growth of described low temperature p-type GaN layer terminates, growth thickness is the PAlGaN electric current resistance of 10nm Barrier, growth temperature is 800 DEG C, and growth time is 2min, and growth pressure is 50Torr, and V/III ratio is 10, in p-type AlGaN layer, the molar constituent content of Al is 5%;
(9), after the growth of described PAlGaN current barrier layer terminates, growth thickness is the high temperature p-type of 100nm GaN layer, growth temperature is 850 DEG C, and growth time is 5min, and growth pressure is 100Torr, V/III ratio It is 300;
(10) described high temperature p-type GaN layer growth terminate after, growth thickness at the p-type contact layer of 5nm, Growth temperature is 850 DEG C, and growth time is 1min, and growth pressure is 100Torr, and V/III ratio is 1000;
(11) after epitaxial growth terminates, the temperature of reative cell is down to 650-800 DEG C, uses pure nitrogen gas gas Atmosphere carries out making annealing treatment 2min, is then down to room temperature, subsequently, after over cleaning, deposition, photoetching and etching Continuous processing technique makes single small-size chips.
In the present embodiment with trimethyl gallium (TMGa), triethyl-gallium (TEGa), trimethyl aluminium (TMAl), three Methyl indium (TMIn) and ammonia (NH3) respectively as Ga, Al, In and N source;With silane (SiH4) and Two cyclopentadienyl magnesium (CP2Mg) respectively as N, P-type dopant, with hydrogen (H2) as carrier gas.
Embodiment 2
A kind of GaN base LED multi-level buffer layer growth method with Sapphire Substrate as substrate, its multi-level buffer layer Epitaxial structure, order from bottom to top includes successively: substrate, multistage LT-AlGaN/MT-GaN/HT-GaN are slow Rush layer, GaN non-doped layer, N-type GaN layer, shallow quantum well layer, luminescent quantum well layer, low temperature p-type GaN Layer, PAlGaN current barrier layer, high temperature p-type GaN layer, p-type contact layer, the growing method of its epitaxial structure Including step in detail below:
(1) substrate is carried out in 1200 DEG C of hydrogen atmospheres high-temperature cleaning and processes 20min, then nitrogenize Process, the outer sapphire material of substrate;
(2) drop to 600 DEG C at a temperature of inciting somebody to action, adjust the preparation growth of epitaxial growth atmosphere multistage LT-AlGaN/MT-GaN/HT-GaN cushion, described multistage LT-AlGaN/MT-GaN/HT-GaN cushion bag Include multiple LT-AlGaN/MT-GaN/HT-GaN structure overlapping successively, at high temperature through H2Processed is blue precious Stone grown on substrates AlGaN layer is 600 DEG C, epitaxial growth under the conditions of reaction cavity pressure 500Torr, thick Degree is 30nm;After AlGaN layer has grown, temperature is increased to 1100 DEG C and carries out thermal anneal process;Afterwards, MT-GaN layer 950 DEG C, enter with 10.0 μm/h high development speed under the conditions of reaction cavity pressure 400Torr Row epitaxial growth, thickness is 2 μm;HT-GaN layer is 1080 DEG C, reaction cavity pressure 200Torr in temperature Under the conditions of carry out epitaxial growth with the low growth rate of 4.0 μm/h, thickness is 2 μm, finally at 1010 DEG C of bars Through H under part2Gas disposal epitaxial surface, prepares growth next cycle, multistage LT-AlGaN/MT-GaN/HT-GaN Buffer layer structure 20 cycles of overlapping growth successively;
(3), after described multistage LT-AlGaN/MT-GaN/HT-GaN buffer growth terminates, temperature is regulated To 1200 DEG C, epitaxial growth thickness is the GaN non-doped layer of 2 μm, and growth pressure is 300Torr, V/ III ratio is 3000;
(4) after the growth of described GaN non-doped layer terminates, the N-type GaN layer that growth doping content is stable is thick Degree is 8.4 μm, and growth temperature is 1200 DEG C, and pressure is 600Torr, and V/III ratio is 3000;
(5) after the growth of described N-type GaN layer terminates, growing shallow quantum well layer, described shallow quantum well layer includes 15 quantum well structures overlapping successively, growth temperature is 920 DEG C, and growth pressure is 500Torr, V/III Ratio is 5000, and thickness is 200nm;
(6) after the growth of described shallow quantum well layer terminates, growing luminescent layer multiple quantum well layer, growth temperature is 850 DEG C, growth pressure is 500Torr, and V/III mol ratio is 5000, described luminescent layer MQW by The In in 12 cyclesyGa1-yN (x < y < 1)/GaN MQW composition, described InyGa1-yN (x < y < 1) SQW Layer thickness is 5nm, and growth temperature is 820 DEG C;Described GaN barrier layer thickness is 15nm, and growth temperature is 920 DEG C, Growth pressure is 500Torr, and V/III mol ratio is 5000;
(7), after the growth of described luminescent layer quantum well layer terminates, growth thickness is low temperature p-type GaN of 100nm Layer, growth temperature is 820 DEG C, and growth time is 35min, and growth pressure is 500Torr, and V/III ratio is 5000;
(8), after the growth of described low temperature p-type GaN layer terminates, growth thickness is the PAlGaN electric current of 200nm Barrier layer, growth temperature is 1200 DEG C, and growth time is 18min, and growth pressure is 500Torr, V/III Ratio is 1000, and in p-type AlGaN layer, the molar constituent content of Al is 30%;
(9), after the growth of described PAlGaN current barrier layer terminates, growth thickness is the high temperature p-type of 800nm GaN layer, growth temperature is 950 DEG C, and growth time is 40min, and growth pressure is 500Torr, V/III ratio It is 5000;
(10), after the growth of described high temperature p-type GaN layer terminates, growth thickness is the p-type contact layer of 20nm, Growth temperature is 1050 DEG C, and growth time is 10min, and growth pressure is 500Torr, and V/III ratio is 20000;
(11) after epitaxial growth terminates, the temperature of reative cell is down to 800 DEG C, uses pure nitrogen gas atmosphere to enter Row annealing 15min, is then down to room temperature, subsequently, adds through over cleaning, deposition, photoetching and etching are follow-up Work technique makes single small-size chips.
In the present embodiment with trimethyl gallium (TMGa), triethyl-gallium (TEGa), trimethyl aluminium (TMAl), three Methyl indium (TMIn) and ammonia (NH3) respectively as Ga, Al, In and N source;With silane (SiH4) and Two cyclopentadienyl magnesium (CP2Mg) respectively as N, P-type dopant, with hydrogen (H2) as carrier gas.
Embodiment 3
A kind of GaN base LED multi-level buffer layer growth method with Sapphire Substrate as substrate, its multi-level buffer layer Epitaxial structure, order from bottom to top includes successively: substrate, multistage LT-AlGaN/MT-GaN/HT-GaN are slow Rush layer, GaN non-doped layer, N-type GaN layer, shallow quantum well layer, luminescent quantum well layer, low temperature p-type GaN Layer, PAlGaN current barrier layer, high temperature p-type GaN layer, p-type contact layer, the growing method of its epitaxial structure Including step in detail below:
(1) substrate is carried out in 1100 DEG C of hydrogen atmospheres high-temperature cleaning and processes 10min, then nitrogenize Process, the outer sapphire material of substrate;
(2) drop to 600 DEG C at a temperature of inciting somebody to action, adjust the preparation growth of epitaxial growth atmosphere multistage LT-AlGaN/MT-GaN/HT-GaN cushion, described multistage LT-AlGaN/MT-GaN/HT-GaN cushion bag Include multiple LT-AlGaN/MT-GaN/HT-GaN structure overlapping successively, at high temperature through H2Processed is blue precious Stone grown on substrates AlGaN layer is 600 DEG C, epitaxial growth under the conditions of reaction cavity pressure 500Torr, thick Degree is 20nm;After AlGaN layer has grown, temperature is increased to 1050 DEG C and carries out thermal anneal process;Afterwards, MT-GaN layer 950 DEG C, carry out with 5.0 μm/h high development speed under the conditions of reaction cavity pressure 400Torr Epitaxial growth, thickness is 1 μm;HT-GaN layer is 1080 DEG C, reaction cavity pressure 200Torr bar in temperature Carrying out epitaxial growth with the low growth rate of 3.0 μm/h under part, thickness is 1 μm, finally 1000 DEG C of conditions Lower through H2Gas disposal epitaxial surface, prepares growth next cycle, multistage LT-AlGaN/MT-GaN/HT-GaN Buffer layer structure 15 cycles of overlapping growth successively;
(3), after described multistage LT-AlGaN/MT-GaN/HT-GaN buffer growth terminates, temperature is regulated To 1100 DEG C, epitaxial growth thickness is the GaN non-doped layer of 1 μm, and growth pressure is 200Torr, V/ III ratio is 1000;
(4) after the growth of described GaN non-doped layer terminates, the N-type GaN layer that growth doping content is stable is thick Degree is 5.0 μm, and growth temperature is 1100 DEG C, and pressure is 500Torr, and V/III ratio is 2000;
(5) after the growth of described N-type GaN layer terminates, growing shallow quantum well layer, described shallow quantum well layer includes 12 quantum well structures overlapping successively, growth temperature is 850 DEG C, and growth pressure is 400Torr, V/III Ratio is 4000, and thickness is 100nm;
(6) after the growth of described shallow quantum well layer terminates, growing luminescent layer multiple quantum well layer, growth temperature is 800 DEG C, growth pressure is 400Torr, and V/III mol ratio is 4000, described luminescent layer MQW by The In in 10 cyclesyGa1-yN (x < y < 1)/GaN MQW composition, described InyGa1-yN (x < y < 1) SQW Layer thickness is 4nm, and growth temperature is 800 DEG C;Described GaN barrier layer thickness is 10nm, and growth temperature is 900 DEG C, Growth pressure is 300Torr, and V/III mol ratio is 3000;
(7), after the growth of described luminescent layer quantum well layer terminates, growth thickness is low temperature p-type GaN of 50nm Layer, growth temperature is 720 DEG C, and growth time is 30min, and growth pressure is 400Torr, and V/III ratio is 3000;
(8), after the growth of described low temperature p-type GaN layer terminates, growth thickness is the PAlGaN electric current of 100nm Barrier layer, growth temperature is 1000 DEG C, and growth time is 15min, and growth pressure is 400Torr, V/III Ratio is 500, and in p-type AlGaN layer, the molar constituent content of Al is 25%;
(9), after the growth of described PAlGaN current barrier layer terminates, growth thickness is the high temperature p-type of 500nm GaN layer, growth temperature is 900 DEG C, and growth time is 30min, and growth pressure is 300Torr, V/III ratio It is 1000;
(10), after the growth of described high temperature p-type GaN layer terminates, growth thickness is the p-type contact layer of 10nm, Growth temperature is 950 DEG C, and growth time is 5min, and growth pressure is 400Torr, and V/III ratio is 10000;
(11) after epitaxial growth terminates, the temperature of reative cell is down to 700 DEG C, uses pure nitrogen gas atmosphere to enter Row annealing 10min, is then down to room temperature, subsequently, adds through over cleaning, deposition, photoetching and etching are follow-up Work technique makes single small-size chips.
In the present embodiment with trimethyl gallium (TMGa), triethyl-gallium (TEGa), trimethyl aluminium (TMAl), three Methyl indium (TMIn) and ammonia (NH3) respectively as Ga, Al, In and N source;With silane (SiH4) and Two cyclopentadienyl magnesium (CP2Mg) respectively as N, P-type dopant, with hydrogen (H2) as carrier gas.
The present invention by multistage LT-AlGaN/MT-GaN/HT-GaN buffer layer structure preferably solve sapphire with Macrolattice mismatch problem between GaN, can reduce the stress between sapphire and GaN, reduces threading dislocation, Improve crystal mass, reduce electric leakage;Meanwhile, this kind of growing method can be periodically during alternating growth Progressively bury in oblivion the threading dislocation produced with GaN interface from substrate, reduce threading dislocation further, thus subtract The non-radiative recombination center of rare source region, improves the brightness of epitaxial wafer, improves LED luminous efficiency.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described.The industry Skilled person will appreciate that, the present invention is not restricted to the described embodiments, in above-described embodiment and description The principle that the present invention is simply described described, without departing from the spirit and scope of the present invention, the present invention Also having various changes and modifications, these changes and improvements both fall within scope of the claimed invention.This The claimed scope of invention is defined by appending claims and equivalent thereof.

Claims (4)

1. the GaN base LED multi-level buffer layer growth method with Sapphire Substrate as substrate, it is multistage slow Rushing layer epitaxial structure, order from bottom to top includes successively: substrate, multistage LT-AlGaN/MT-GaN/HT-GaN Cushion, GaN non-doped layer, N-type GaN layer, shallow quantum well layer, luminescent quantum well layer, low temperature p-type GaN Layer, PAlGaN current barrier layer, high temperature p-type GaN layer, p-type contact layer, it is characterised in that: its epitaxy junction The growing method of structure includes step in detail below:
(1) substrate is carried out in 1000-1200 DEG C of hydrogen atmosphere high-temperature cleaning and processes 5-20min, then Carrying out nitrogen treatment, substrate is sapphire material;
(2) drop to 600 DEG C at a temperature of inciting somebody to action, adjust the preparation growth of epitaxial growth atmosphere multistage LT-AlGaN/MT-GaN/HT-GaN cushion, described multistage LT-AlGaN/MT-GaN/HT-GaN cushion bag Include multiple LT-AlGaN/MT-GaN/HT-GaN structure overlapping successively, at high temperature through H2Processed is blue precious Stone grown on substrates AlGaN layer is 600 DEG C, epitaxial growth under the conditions of reaction cavity pressure 500Torr, thick Degree is 10-30nm;After AlGaN layer has grown, temperature is increased to 1010-1100 DEG C and carries out at thermal annealing Reason;Afterwards, MT-GaN layer 950 DEG C, under the conditions of reaction cavity pressure 400Torr with 4.0-10.0 μm/h High development speed carries out epitaxial growth, and thickness is 0.2-2 μm;HT-GaN layer temperature be 1080 degree, anti- Carrying out epitaxial growth with 2.0-4.0 μm/low growth rate of h under the conditions of answering chamber pressure 200Torr, thickness is 0.1-2 μm, finally through H under the conditions of 1000-1010 DEG C2Gas disposal epitaxial surface, prepares growth next week Phase, multistage LT-AlGaN/MT-GaN/HT-GaN buffer layer structure 2-20 the cycle of overlapping growth successively;
(3), after described multistage LT-AlGaN/MT-GaN/HT-GaN buffer growth terminates, temperature is regulated To 1000-1200 DEG C, epitaxial growth thickness is the GaN non-doped layer of 0.5-2 μm, and growth pressure is 100-300Torr, V/III ratio is 100-3000;
(4) after the growth of described GaN non-doped layer terminates, the N-type GaN layer that growth doping content is stable is thick Degree is 2.4-8.4 μm, and growth temperature is 1000-1200 DEG C, and pressure is 100-600Torr, and V/III ratio is 100-3000;
(5) after the growth of described N-type GaN layer terminates, growing shallow quantum well layer, described shallow quantum well layer includes 3-15 quantum well structure overlapping successively, growth temperature is 820-920 DEG C, and growth pressure is 100-500Torr, V/III ratio is 300-5000, and thickness is 10-200nm;
(6) after the growth of described shallow quantum well layer terminates, growing luminescent layer multiple quantum well layer, growth temperature is 700-850 DEG C, growth pressure is 100-500Torr, and V/III mol ratio is 300-5000, described luminescence Layer MQW is by the In in 6-12 cycleyGa1-yN/GaN wherein x < y < 1, MQW forms, described InyGa1-yN, wherein x < y < 1, quantum well layer thickness is 2-5nm, and growth temperature is 720-820 DEG C;Described GaN barrier layer thickness is 8-15nm, and growth temperature is 820-920 DEG C, and growth pressure is 100-500Torr, V/III mol ratio is 300-5000;
(7), after the growth of described luminescent layer quantum well layer terminates, growth thickness is the low temperature p-type of 10-100nm GaN layer, growth temperature is 620-820 DEG C, and growth time is 5-35min, and growth pressure is 100-500Torr, V/III ratio is 300-5000;
(8), after the growth of described low temperature p-type GaN layer terminates, growth thickness is the PAlGaN electricity of 10-200nm Flow barrier, growth temperature is 800-1200 DEG C, and growth time is 2-18min, and growth pressure is 50-500Torr, V/III ratio is 10-1000, and in p-type AlGaN layer, the molar constituent content of Al is 5%~30%;
(9), after the growth of described PAlGaN current barrier layer terminates, growth thickness is the high temperature P of 100-800nm Type GaN layer, growth temperature is 850-950 DEG C, and growth time is 5-40min, and growth pressure is 100-500Torr, V/III ratio is 300-5000;
(10), after the growth of described high temperature p-type GaN layer terminates, growth thickness is the p-type contact of 5-20nm Layer, growth temperature is 850-1050 DEG C, and growth time is 1-10min, and growth pressure is 100-500Torr, V/III ratio is 1000-20000;
(11) after epitaxial growth terminates, the temperature of reative cell is down to 650-800 DEG C, uses pure nitrogen gas gas Atmosphere carries out making annealing treatment 2-15min, is then down to room temperature, subsequently, through over cleaning, deposition, photoetching and etching Subsequent machining technology makes single small-size chips.
A kind of GaN base LED multi-level buffer with Sapphire Substrate as substrate the most according to claim 1 Layer growth method, it is characterised in that: in the growth course of described epitaxial structure with trimethyl gallium (TMGa), three Ethyl gallium (TEGa), trimethyl aluminium (TMAl), trimethyl indium (TMIn) and ammonia (NH3) respectively as Ga, Al, In and N source.
A kind of GaN base LED multi-level buffer with Sapphire Substrate as substrate the most according to claim 1 Layer growth method, it is characterised in that: with silane (SiH in the growth course of described epitaxial structure4) and two cyclopentadienyl magnesium (CP2Mg) respectively as N, P-type dopant.
A kind of GaN base LED multi-level buffer with Sapphire Substrate as substrate the most according to claim 1 Layer growth method, it is characterised in that: with hydrogen (H in the growth course of described epitaxial structure2) or nitrogen (N2) As carrier gas.
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