CN106299041A - The preparation method and application of the nonpolar LED being grown in r surface sapphire substrate - Google Patents

The preparation method and application of the nonpolar LED being grown in r surface sapphire substrate Download PDF

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CN106299041A
CN106299041A CN201610754992.6A CN201610754992A CN106299041A CN 106299041 A CN106299041 A CN 106299041A CN 201610754992 A CN201610754992 A CN 201610754992A CN 106299041 A CN106299041 A CN 106299041A
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nonpolar
sapphire substrate
gan
surface sapphire
led
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李国强
杨为家
王文樑
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South China University of Technology SCUT
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South China University of Technology SCUT
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Priority to PCT/CN2016/098634 priority patent/WO2018040124A1/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005Processes
    • 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
    • H01L33/007Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02367Substrates
    • H01L21/02433Crystal orientation
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02612Formation types
    • H01L21/02617Deposition types
    • H01L21/0262Reduction or decomposition of gaseous compounds, e.g. CVD
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/12Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a stress relaxation structure, e.g. buffer layer

Abstract

The invention discloses the preparation method of the nonpolar LED being grown in r surface sapphire substrate, comprise the following steps: (1) uses r surface sapphire substrate, chooses crystal orientation;(2) r surface sapphire substrate is carried out surface cleaning process;(3) the r surface sapphire substrate after step (2) being processed transfers to the ultrahigh vacuum growth room growing nonpolar GaN cushion of pulsed laser deposition equipment;(4) MOCVD technique epitaxial lateral overgrowth nonpolar undoped u GaN layer is used;(5) MOCVD technique growing nonpolar N-shaped doping GaN film is used;(6) MOCVD technique growing nonpolar InGaN/GaN SQW is used;(7) MOCVD technique growing nonpolar p-type doping GaN film is used.The preparation method that the present invention proposes has that technique is simple, time-saving and efficiency, can increase substantially the features such as film crystal quality and device performance.

Description

The preparation method of the nonpolar LED being grown in r surface sapphire substrate and Application
Technical field
The present invention relates to nonpolar LED, particularly to being grown in outside the nonpolar LED in r surface sapphire substrate Prolong the preparation method and application of sheet.
Background technology
Light emitting diode (LED), as a kind of novel solid lighting source and green light source, has that volume is little, power consumption Low, environmental protection, length in service life, high brightness, the outstanding feature such as low in calories and colorful, at outdoor lighting, commercial lighting and dress The fields such as decorations engineering all have a wide range of applications.Currently, in the background that global warming and lack of energy problem are increasingly severe Under, save the energy, reduce greenhouse gas emission become the whole world common faced by major issue.With low energy consumption, low stain, low emission Based on low-carbon economy, the important directions of economic development will be become.At lighting field, the application of LED luminous product just attracts The sight of common people, LED is as a kind of novel green light source product, the necessarily trend of future development, and 21st century will It it is the epoch of novel illumination light source with LED as representative.But the application cost of present stage LED is higher, and luminous efficiency is relatively low, this A little factors all can significantly limit LED and develop to the direction of high-efficient energy-saving environment friendly.
The luminous efficiency of LED chip is not high enough is the key issue limiting LED development, and it is primarily due to mesh Front widely used GaN base LED all grows along polarity c-axis.On c-axis direction, Ga atom set and the barycenter of atom N set Misaligned, thus form electric dipole, produce spontaneous polarization field and piezoelectric polarization fields, and then cause quantum to fetter Stark effect (Quantum-confined Starker Effect, QCSE), makes electronics separate with hole, the radiation recombination efficiency of carrier Reduce, finally affect the luminous efficiency of LED, and cause the instability of LED emission wavelength.Solving this problem best bet is Non-polar GaN material is used to make LED, to eliminate the impact of quantum constraint Stark effect.Theoretical research shows, uses non-pole Property GaN manufacture LED, can make LED luminous efficiency improve by about one time.
As can be seen here, LED to be made really realizes extensive extensively application, improves the luminous efficiency of LED chip, and reduces it Manufacturing cost, the most basic way researches and develops non-polar GaN-based LED epitaxial chip exactly on low cost, large scale Novel substrate. At present, the representative of the Novel substrate preparing nonpolar GaN film mainly has r surface sapphire, r surface sapphire, LiAlO2Deng.With it Its substrate is compared, and r surface sapphire substrate has three below considerable advantage.First, sapphire preparation technology becomes the most very much Ripe.Second, large-size sapphire substrate has been tested and has been commercially produced, and relatively cheap this of price is industrialized production Establish solid foundation.3rd, the preparation technology of Sapphire Substrate LED is the most highly developed and perfect, once r surface sapphire On substrate, nonpolar LED makes a breakthrough, and it just can realize rapidly industrialization and produce, and creates substantial amounts of economic benefit and society's effect Benefit.But, r surface sapphire substrate is relatively big (16%) with the lattice mismatch of GaN, uses metal-organic chemical vapor deposition equipment (MOCVD) or molecular beam epitaxy (MBE) the most easily grows polycrystalline state GaN, and need under bigger thickness (generally More than 3 μm) high-quality nonpolar GaN film could be obtained.
Pulsed laser deposition (PLD) overcomes the deficiency of MOCVD, MBE and the problem of existence.Its major advantage has following Several aspects: (1) laser energy density is high, can be deposited with the various target being difficult to and melting, it is achieved the low-temperature epitaxy growth of thin film, Effectively suppress interfacial reaction;(2) technological parameter is easy to adjust, and sedimentation rate is high, and experimental period is short;(3) development potentiality is big, tool There is good compatibility;(4) thin film composition is stable, it is easy to obtain desired stoichiometric proportion;(5) multiple target can be placed simultaneously Material (4-6), the plural layers that beneficially prepared composition is complicated;(6) cleaning processes very convenient, can prepare different types of Thin film.Generally speaking, PLD can prepare high quality monocrystalline film (less than 1 μm) under less thickness.But, anything All there is dual character in thing.The major defect of PLD is exactly that sedimentation rate is high, it is difficult to the SQW of preparation high-quality.It is true that quantum Well structure LED has become as one of Main Trends of The Development of following LED.This shortcoming of PLD, seriously limit it popularization and Range of application.
Summary of the invention
In order to overcome the disadvantages mentioned above of prior art with not enough, it is an object of the invention to provide one and be grown in r face indigo plant The preparation method of the nonpolar LED on gem substrate, prepare be grown in r surface sapphire substrate nonpolar LED has the features such as defect concentration is low, crystalline quality is good.
The nonpolar LED that another object of the present invention is to provide above-mentioned length in r surface sapphire substrate should With.
The purpose of the present invention is achieved through the following technical solutions:
The preparation method of the nonpolar LED being grown in r surface sapphire substrate, comprises the following steps:
(1) use r surface sapphire substrate, choose crystal orientation;
(2) r surface sapphire substrate is carried out surface cleaning process;
(3) the r surface sapphire substrate after step (2) being processed transfers to the ultrahigh vacuum growth of pulsed laser deposition equipment Room, growing nonpolar GaN cushion, form horizontal extension district, process conditions are: underlayer temperature rises to 250~550 DEG C, use Pulsed laser ablation GaN target, is passed through N simultaneously2Plasma, chamber pressure is 1-20mTorr, laser energy be 150~ 400mJ, laser frequency is 2~30Hz;
(4) using MOCVD technique epitaxial lateral overgrowth nonpolar undoped u-GaN layer, process conditions are: underlayer temperature Being 950~1100 DEG C, be passed through TMGa, chamber pressure is 80~200Torr, and V/III ratio is 80~150;
(5) use MOCVD technique growing nonpolar N-shaped doping GaN film, process conditions are: underlayer temperature be 1000~ 1100 DEG C, it is passed through TGGa and SiH4, keep SiH4Flow be 60~90sccm, chamber pressure is 80~200Torr, V/III Ratio is 80~150;Doping electron concentration 1.0 × 1017~6.0 × 1019cm-3
(6) using MOCVD technique growing nonpolar InGaN/GaN SQW, process conditions are: barrier layer, and underlayer temperature is 750~850 DEG C, close H2, it being passed through TEGa and ammonia, chamber pressure is 200Torr, and V/III ratio is 500~1500, thickness It is 10~13nm;Well layer, underlayer temperature is 750~850 DEG C, closes H2, it being passed through TEGa, TMIn and ammonia, chamber pressure is 80~200Torr, V/III ratio is 500~1500, and thickness is 2~3nm;
(7) use MOCVD technique growing nonpolar p-type doping GaN film, process conditions are: underlayer temperature be 900~ 1050 DEG C, it is passed through TMGa, CP2Mg and ammonia, keep CP2The flow of Mg is 250~450sccm, chamber pressure be 80~ 200Torr, V/III ratio is 950~1150;Doping hole concentration 1.0 × 1016~4.0 × 1018cm-3
The thickness of described nonpolar low temperature GaN buffer is 150~500nm.
The thickness of described nonpolar undoped u-GaN layer is 2850~3500nm.
The thickness of described nonpolar N-shaped doping GaN film is 300~700nm.
Described nonpolar InGaN/GaN SQW is the InGaN well layer/GaN barrier layer, wherein InGaN trap in 5~10 cycles The thickness of layer is 2~3nm;The thickness of GaN barrier layer is 10~13nm.
The thickness of described nonpolar p-type doping GaN film is 350~500nm.
Step (2) is described carries out surface cleaning process to r surface sapphire substrate, particularly as follows:
R surface sapphire substrate is put in deionized water under room temperature ultrasonic cleaning 5~10 minutes, removes r surface sapphire lining Basal surface pickup granule, then sequentially pass through washing with alcohol, remove surface organic matter;R surface sapphire substrate after cleaning is with high-purity Drying nitrogen dries up;Afterwards r surface sapphire substrate is put into PLD growth room, under vacuum, underlayer temperature is risen to 850 ~900 DEG C, toast 20~30 minutes, remove the impurity of r surface sapphire substrate surface residual, then pass to N2 plasma, protect Temperature 30~60 minutes, makes substrate surface form AlN inculating crystal layer, provides template for GaN growth.
Step chooses crystal orientation described in (1), particularly as follows: inclined 0.2 ° of (1-100) direction is as epitaxial surface with (10-12) face, Crystalline epitaxial orientation relationship is: (0001) face of GaN is parallel to (-1011) face of r surface sapphire.
The growth that the preparation method of the described nonpolar LED being grown in r surface sapphire substrate prepares The application of the nonpolar LED in r surface sapphire substrate, it is characterised in that be used for preparing LED, LD, photodetector And solaode.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) present invention is first by PLD high-quality GaN cushion of low-temperature epitaxy one layer on substrate, is formed graphical Vitellarium (template), the epitaxial lateral overgrowth for follow-up MOCVD provides condition;Then MOCVD epitaxial lateral overgrowth is used U-GaN, then extension n-GaN, SQW, p-GaN etc..The present invention is conducive to preparing high-quality nonpolar GaN film, has The features such as defect concentration is low, crystalline quality is good, can be widely applied to the fields such as LED, LD, solaode.
(2) preparation method that the present invention proposes has that technique is simple, the advantage of time-saving and efficiency.
Accompanying drawing explanation
Fig. 1 is the epitaxial structure generalized section of the nonpolar LED of embodiment 1 preparation.
Fig. 2 is the XRD scanning spectra of the non-polar GaN cushion of embodiment 1 preparation.
X-ray Rocking Curve (XRC) collection of illustrative plates of non-polar GaN cushion prepared by Fig. 3.
Fig. 4 is the AFM picture of the non-polar GaN cushion of embodiment 1 preparation.
Fig. 5 is luminescence generated by light (PL) collection of illustrative plates of the nonpolar LED of embodiment 1 preparation.
Fig. 6 is electroluminescent (EL) collection of illustrative plates of the nonpolar LED of embodiment 1 preparation.
Fig. 7 is the luminous power-electric current collection of illustrative plates of the nonpolar LED of embodiment 1 preparation.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
The preparation method of the nonpolar LED being grown in r surface sapphire substrate, comprises the following steps:
1) the choosing of substrate and its crystal orientation: use r surface sapphire substrate, with 0.2 ° of (1-100) direction partially, (10-12) face For epitaxial surface, crystalline epitaxial orientation relationship is: (0001) face of GaN is parallel to (-1011) face of r surface sapphire.
2) substrate cleans and annealing, and described cleaning, particularly as follows: put into r surface sapphire substrate in deionized water Ultrasonic cleaning 3 minutes under room temperature, remove r surface sapphire substrate surface pickup granule, then through washing with alcohol, remove surface organic Thing, dries up with high-purity drying nitrogen.
Described annealing, particularly as follows: put into PLD growth room by r surface sapphire substrate, under vacuum, by substrate Temperature rises to 900 DEG C, high-temperature baking 20 minutes, removes the impurity of r surface sapphire substrate surface residual, then passes to N2Plasma Body, is incubated 60 minutes, makes substrate surface form AlN inculating crystal layer, provides template for GaN growth.
3) the r surface sapphire substrate carrying out processing is transferred to the ultrahigh vacuum growth room of pulsed laser deposition equipment, Growth 300nm non-polar GaN cushion, forms horizontal extension district, and process conditions are: underlayer temperature rises to 350 DEG C, uses pulse Laser bombardment high-purity GaN (99.99%) target, is passed through N simultaneously2Plasma, chamber pressure is 8mTorr, laser energy is 220mJ, laser frequency is 20Hz;
4) using MOCVD technique epitaxial lateral overgrowth nonpolar undoped u-GaN layer, process conditions are: underlayer temperature Being 1000 DEG C, be passed through TMGa, chamber pressure is 200Torr, and V/III ratio is 120;
5) using MOCVD technique growing nonpolar N-shaped doping GaN film, process conditions are: underlayer temperature is 1050 DEG C, It is passed through TGGa and SiH4, keep SiH4Flow be 60~90sccm, chamber pressure is 200Torr, and V/III ratio is 150.
6) using MOCVD technique growing nonpolar InGaN/GaN SQW, process conditions are: barrier layer, and underlayer temperature is 750 DEG C, close H2, it being passed through TEGa and ammonia, chamber pressure is 200Torr, and V/III ratio is 966;Well layer, underlayer temperature is 750 DEG C, close H2, it being passed through TEGa, TMIn and ammonia, chamber pressure is 200Torr, and V/III ratio is 1439;
7) using MOCVD technique growing nonpolar p-type doping GaN film, process conditions are: underlayer temperature is 950 DEG C, logical Enter TMGa, CP2Mg and ammonia, the flow keeping CP2Mg is 300sccm, and chamber pressure is 200Torr, and V/III ratio is 1050。
As it is shown in figure 1, the nonpolar LED being grown in r surface sapphire substrate of the present embodiment, it includes r surface sapphire Substrate 11, the non-polar GaN cushion 12 being grown in successively in r surface sapphire substrate, nonpolar undoped u-GaN layer 13, non- Polarity N-shaped doping GaN film 14, nonpolar InGaN/GaN SQW 15, nonpolar p-type doping GaN film 16.
Fig. 2 is the XRD scanning spectra of non-polar GaN cushion.As in figure 2 it is shown, thin film only occurs in that Sapphire Substrate Peak and single GaN (11-20) thin film diffraction peak.This explanation, we have prepared non-polar GaN in r surface sapphire substrate Monocrystal thin films.Further test shows, GaN (11-20) the Rocking Curve half-peak of non-polar GaN cushion is a width of 0.8°.This explanation, non-polar GaN cushion has good crystal mass, follow-up high-quality nonpolar GaN film Growth.
Fig. 3 is the XRC collection of illustrative plates of non-polar GaN cushion prepared by the present embodiment.A width of 0.3 ° of the half-peak of XRC, this explanation, Non-polar GaN cushion has good crystal mass, follow-up nonpolar GaN film and the preparation of device.
Fig. 4 is the AFM picture of non-polar GaN cushion prepared by the present embodiment.As it is shown on figure 3, non-polar GaN cushion Having well-regulated strip pattern, it as graphical template, can promote the two-dimensional transversal epitaxial lateral overgrowth of MOCVD, favorably In the quality of raising thin film, solid foundation has been established in the preparation for the nonpolar LED of high-quality.
Fig. 5 is the PL collection of illustrative plates of nonpolar LED prepared by the present embodiment.As shown in Figure 4, nonpolar LED occurs at 446nm Strong excitation peak, a width of 22nm of its half-peak.The respective value of this numerical value commercialization to be much better than LED.This shows, nonpolar LED has good photoelectric properties.
Fig. 6 is the EL collection of illustrative plates of nonpolar LED prepared by the present embodiment.As it is shown in figure 5, nonpolar LED occurs at 444nm Strong excitation peak, a width of 20.4nm of its half-peak.The respective value of this numerical value commercialization to be much better than LED.This shows, non-pole Property LED have excellence photoelectric properties.
Fig. 7 is the luminous power-electric current collection of illustrative plates of nonpolar LED prepared by the present embodiment.From the figure, it can be seen that luminous power with The increasing of electric current to and increase rapidly.Optical output power under 100mA is 22.5mW.It is indicated above that nonpolar LED has excellence Electric property.
The nonpolar LED that prepared by the present embodiment be grown in r surface sapphire substrate, includes that non-polar GaN buffers successively Layer, the N-shaped of undoped u-GaN thin film, Si doping mix silicon GaN, InxGa1-xThe p-type of N multiple quantum well layer, Mg doping mixes the GaN of magnesium Layer.The GaN base LED component prepared in r surface sapphire substrate, the thickness of its N-shaped GaN is about 450nm, its carrier Concentration is 2.7 × 1019cm-3;InxGa1-xThe thickness of N/GaN multiple quantum well layer is about 150nm, and periodicity is 8, wherein InxGa1- xN well layer be 2nm, GaN barrier layer be 12nm, p-type is mixed the GaN layer thickness of magnesium and is about 300nm, the concentration of its carrier is 5.5 × 1017cm-3.Under the operating current of 20mA, the optical output power of LED component is 7.3mW, and cut-in voltage value is 3.00V.
The nonpolar GaN film being grown in r surface sapphire substrate prepared by the present embodiment is used for preparing photodetection Device: epitaxial growth N-shaped mixes silicon GaN, non-successively in the GaN film being grown in r surface sapphire substrate prepared by the present embodiment Doping GaN, p-type mix the GaN of magnesium, and last electron beam evaporation forms Ohmic contact and schottky junction.Wherein N-shaped mixes silicon GaN thickness Being about 3 μm, the concentration of its carrier is 2.9 × 1019cm-3;Undoped GaN thickness is about 300nm, and its carrier concentration is 3.4 ×1016cm-3;P-type is mixed the GaN degree of magnesium and is about 1.8 μm.Photodetector prepared by the present embodiment 1V bias under, dark current Being only 40pA, and device is under 1V biases, at 356nm, the maximum of responsiveness has reached 1.7A/W.
The GaN film being grown in r surface sapphire substrate prepared by the present embodiment is used for preparing InGaN solar-electricity Pond: growth has component gradient successively in the GaN film being grown in r surface sapphire substrate prepared by the present embodiment InxGa1-xN cushion, N-shaped mixes silicon InxGa1-xN,InxGa1-xN multiple quantum well layer, p-type mixes the In of magnesiumxGa1-xN shell, last electronics Beam evaporation forms Ohmic contact, wherein 0 < x≤0.2.Wherein, N-shaped mixes silicon InxGa1-xN thickness is about 5.5 μm, its carrier Concentration is 2.4 × 1019cm-3;InxGa1-xN multiple quantum well layer, thickness is about 400nm, and periodicity is 20, wherein In0.2Ga0.8N trap Layer is 3nm, In0.08Ga0.92N barrier layer is 12nm.Electricity conversion under the solaode room temperature that this technique prepares is 10.2%, circuit photocurrent density is 32mA/cm2
Embodiment 2
The preparation method of the nonpolar LED being grown in r surface sapphire substrate, comprises the following steps:
1) the choosing of substrate and its crystal orientation: use r surface sapphire substrate, with 0.2 ° of (1-100) direction partially, (10-12) face For epitaxial surface, crystalline epitaxial orientation relationship is: (0001) face of GaN is parallel to (-1011) face of r surface sapphire.
2) substrate cleans and annealing, and described cleaning, particularly as follows: put into r surface sapphire substrate in deionized water Ultrasonic cleaning 3 minutes under room temperature, remove r surface sapphire substrate surface pickup granule, then through washing with alcohol, remove surface organic Thing, dries up with high-purity drying nitrogen.
Described annealing, particularly as follows: put into PLD growth room by r surface sapphire substrate, under vacuum, by substrate Temperature rises to 850 DEG C, high-temperature baking 30 minutes, removes the impurity of r surface sapphire substrate surface residual, then passes to N2Plasma Body, is incubated 30 minutes, makes substrate surface form AlN inculating crystal layer, provides template for GaN growth.
3) the r surface sapphire substrate carrying out processing is transferred to the ultrahigh vacuum growth room of pulsed laser deposition equipment, Growth 400nm non-polar GaN cushion, forms horizontal extension district, and process conditions are: underlayer temperature rises to 400 DEG C, uses pulse Laser bombardment high-purity GaN (99.99%) target, is passed through N simultaneously2Plasma, chamber pressure is 20mTorr, laser energy For 250mJ, laser frequency is 20Hz;
4) using MOCVD technique epitaxial lateral overgrowth nonpolar undoped u-GaN layer, process conditions are: underlayer temperature Being 1020 DEG C, be passed through TMGa, chamber pressure is 80Torr, and V/III ratio is 150;
5) using MOCVD technique growing nonpolar N-shaped doping GaN film, process conditions are: underlayer temperature is 1050 DEG C, It is passed through TGGa and SiH4, keep SiH4Flow be 60~90sccm, chamber pressure is 80Torr, and V/III ratio is 80.
6) using MOCVD technique growing nonpolar InGaN/GaN SQW, process conditions are: barrier layer, and underlayer temperature is 750 DEG C, close H2, it being passed through TEGa and ammonia, chamber pressure is 80Torr, and V/III ratio is 1500;Well layer, underlayer temperature is 750 DEG C, close H2, it being passed through TEGa, TMIn and ammonia, chamber pressure is 200Torr, and V/III ratio is 500;
7) using MOCVD technique growing nonpolar p-type doping GaN film, process conditions are: underlayer temperature is 950 DEG C, logical Enter TMGa, CP2Mg and ammonia, the flow keeping CP2Mg is 300sccm, and chamber pressure is 80Torr, and V/III ratio is 950.
The nonpolar LED that prepared by the present embodiment be grown in r surface sapphire substrate, includes that non-polar GaN buffers successively Layer, the N-shaped of undoped u-GaN thin film, Si doping mix silicon GaN, InxGa1-xThe p-type of N multiple quantum well layer, Mg doping mixes the GaN of magnesium Layer.The GaN base LED component prepared in r surface sapphire substrate, the thickness of its N-shaped GaN is about 500nm, its carrier Concentration is 3.0 × 1019cm-3;InxGa1-xThe thickness of N/GaN multiple quantum well layer is about 150nm, and periodicity is 8, wherein InxGa1- xN well layer be 2nm, GaN barrier layer be 12nm, p-type is mixed the GaN layer thickness of magnesium and is about 300nm, the concentration of its carrier is 5.5 × 1017cm-3.Under the operating current of 20mA, the optical output power of LED component is 7.5mW, and cut-in voltage value is 3.00V.
Nonpolar GaN film in r surface sapphire substrate and device prepared by the present embodiment have extraordinary crystal matter Amount and photoelectric properties, test data are close with embodiment 1, do not repeat them here.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by described embodiment Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify, All should be the substitute mode of equivalence, within being included in protection scope of the present invention.

Claims (9)

1. the preparation method of the nonpolar LED being grown in r surface sapphire substrate, it is characterised in that include following step Rapid:
(1) use r surface sapphire substrate, choose crystal orientation;
(2) r surface sapphire substrate is carried out surface cleaning process;
(3) the r surface sapphire substrate after step (2) being processed transfers to the ultrahigh vacuum growth room of pulsed laser deposition equipment, Growing nonpolar GaN cushion, forms horizontal extension district, and process conditions are: underlayer temperature rises to 250~550 DEG C, uses pulse Laser bombardment GaN target, is passed through N simultaneously2Plasma, chamber pressure is 1-20mTorr, laser energy be 150~ 400mJ, laser frequency is 2~30Hz;
(4) using MOCVD technique epitaxial lateral overgrowth nonpolar undoped u-GaN layer, process conditions are: underlayer temperature is 950~1100 DEG C, being passed through TMGa, chamber pressure is 80~200Torr, and V/III ratio is 80~150;
(5) using MOCVD technique growing nonpolar N-shaped doping GaN film, process conditions are: underlayer temperature is 1000~1100 DEG C, it is passed through TGGa and SiH4, keep SiH4Flow be 60~90sccm, chamber pressure is 80~200Torr, and V/III ratio is 80~150;Doping electron concentration 1.0 × 1017~6.0 × 1019cm-3
(6) use MOCVD technique growing nonpolar InGaN/GaN SQW, process conditions are: barrier layer, underlayer temperature be 750~ 850 DEG C, close H2, be passed through TEGa and ammonia, chamber pressure is 200Torr, and V/III ratio is 500~1500, thickness be 10~ 13nm;Well layer, underlayer temperature is 750~850 DEG C, closes H2, be passed through TEGa, TMIn and ammonia, chamber pressure be 80~ 200Torr, V/III ratio is 500~1500, and thickness is 2~3nm;
(7) using MOCVD technique growing nonpolar p-type doping GaN film, process conditions are: underlayer temperature is 900~1050 DEG C, it is passed through TMGa, CP2Mg and ammonia, keep CP2The flow of Mg is 250~450sccm, and chamber pressure is 80~200Torr, V/III ratio is 950~1150;Doping hole concentration 1.0 × 1016~4.0 × 1018cm-3
The preparation method of the nonpolar LED being grown in r surface sapphire substrate the most according to claim 1, its Being characterised by, the thickness of described nonpolar low temperature GaN buffer is 150~500nm.
The preparation method of the nonpolar LED being grown in r surface sapphire substrate the most according to claim 1, its Being characterised by, the thickness of described nonpolar undoped u-GaN layer is 2850~3500nm.
The preparation method of the nonpolar LED being grown in r surface sapphire substrate the most according to claim 1, its Being characterised by, the thickness of described nonpolar N-shaped doping GaN film is 300~700nm.
The preparation method of the nonpolar LED being grown in r surface sapphire substrate the most according to claim 1, its Being characterised by, described nonpolar InGaN/GaN SQW is the InGaN well layer/GaN barrier layer, wherein InGaN in 5~10 cycles The thickness of well layer is 2~3nm;The thickness of GaN barrier layer is 10~13nm.
The preparation method of the nonpolar LED being grown in r surface sapphire substrate the most according to claim 1, its Being characterised by, the thickness of described nonpolar p-type doping GaN film is 350~500nm.
The preparation method of the nonpolar LED being grown in r surface sapphire substrate the most according to claim 1, its Being characterised by, step (2) is described carries out surface cleaning process to r surface sapphire substrate, particularly as follows:
R surface sapphire substrate is put in deionized water under room temperature ultrasonic cleaning 5~10 minutes, removes r surface sapphire substrate table Face pickup granule, then sequentially pass through washing with alcohol, remove surface organic matter;R surface sapphire substrate after cleaning is dried with high-purity Nitrogen dries up;Afterwards r surface sapphire substrate is put into PLD growth room, under vacuum, underlayer temperature is risen to 850~900 DEG C, toast 20~30 minutes, remove the impurity of r surface sapphire substrate surface residual, then pass to N2 plasma, insulation 30~ 60 minutes, make substrate surface form AlN inculating crystal layer, provide template for GaN growth.
The preparation method of the nonpolar LED being grown in r surface sapphire substrate the most according to claim 1, its Being characterised by, step chooses crystal orientation described in (1), particularly as follows: inclined 0.2 ° of (1-100) direction is as epitaxial surface with (10-12) face, Crystalline epitaxial orientation relationship is: (0001) face of GaN is parallel to (-1011) face of r surface sapphire.
9. the preparation side of the nonpolar LED being grown in r surface sapphire substrate described in any one of claim 1~8 The application of the nonpolar LED that what method prepared be grown in r surface sapphire substrate, it is characterised in that be used for preparing LED, LD, photodetector and solaode.
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