CN106067492B - The method that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate - Google Patents
The method that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate Download PDFInfo
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- 229910002601 GaN Inorganic materials 0.000 title claims abstract description 135
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000000758 substrate Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000012010 growth Effects 0.000 claims abstract description 62
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract description 51
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 230000008021 deposition Effects 0.000 claims abstract description 6
- 230000000737 periodic effect Effects 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims description 25
- 230000004888 barrier function Effects 0.000 claims description 23
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 5
- 230000007773 growth pattern Effects 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 description 14
- 230000017525 heat dissipation Effects 0.000 description 6
- 230000035882 stress Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical group C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 1
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0075—Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02387—Group 13/15 materials
- H01L21/02389—Nitrides
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/02428—Structure
- H01L21/0243—Surface structure
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02455—Group 13/15 materials
- H01L21/02458—Nitrides
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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Abstract
The invention discloses a kind of methods that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate, and deposition thickness is the SiO of 98 102nm on gallium nitride monocrystal substrate2Or SiN is as mask pattern layer, the mask pattern layer is prepared as again the round poroid mask pattern layer with periodic structure, a diameter of 0.8 1.0 microns of the circular apertures of the round poroid mask pattern layer, the figure period of the round poroid mask pattern layer is 1.4 1.6 microns, MOCVD reative cells are put into after gallium nitride monocrystal substrate is cleaned up again and carry out diauxic growth, by using reduction MOCVD chamber pressures, improve V/III than mode, control the growth pattern of epitaxial layer of gallium nitride, epitaxial layer can while vertical-growth is continued on mask pattern layer laterally overgrown, prepare high-brightness GaN-based light-emitting diode.Gallium nitride based light emitting diode thermal diffusivity prepared by the present invention is good.
Description
Technical field
The present invention relates to field of semiconductor photoelectron technique, one kind prepares high brightness on graphical gallium nitride monocrystal substrate
The method of gallium nitride light-emitting diode.
Background technology
The heat dissipation of LED is increasingly paid attention to now by people, this is because the light decay of LED or its service life are directly to be tied with it
Temperature is related, and the bad junction temperature that radiates is just high, and the service life often reduces by 10 DEG C of service life with regard to short, according to A Leiniusi rules temperature can extend 2 times.
According to light decay and the relationship of junction temperature, if junction temperature can be controlled at 65 °C, then and the service life of its light decay to 70% can be up to 10
Ten thousand hours！But it is limited to the heat dissipation performance of practical LED light, the service life of LED lamp becomes a master for influencing its performance
Want problem.Moreover, junction temperature not only influences the long-time service life, the luminous efficiency of short time is yet directly affected.For example junction temperature is 25
Luminous quantity when spending is 100%, then when junction temperature rises to 60 degree, luminous quantity just only has 90%；Luminous quantity when junction temperature is 100 degree
Drop down to 80%；Luminous quantity just only has 70% when junction temperature rises to 140 degree.It can be seen that improving the heat dissipation of LED light, junction temperature is controlled
It is highly important thing.In addition to this, the fever of LED can also cause its spectroscopic studying, colour temperature raising, forward current increase
（When constant pressure is powered）, variety of problems that reverse current also increases, and thermal stress increases, and fluorescent material epoxy aging accelerates etc..Cause
This, the heat dissipation of LED be LED lamp design in a mostly important problem.
The characteristics of LED chip is that high heat is generated in minimum volume.Due to the thermal capacity very littles of LED in itself,
So these heats must be conducted with most fast speed, very high junction temperature otherwise will be generated.In order to as much as possible
Heat is drawn out to outside chip, and people have carried out many improvement on the chip structure of LED.In order to improve LED chip in itself
Heat dissipation, most important improvement are exactly using the better substrate material of thermal conductivity.The LED of early stage is only using Si（Silicon）As lining
Bottom.Just being changed to sapphire made substrate later.But the heat conductivility of Sapphire Substrate is not so good.
Invention content
The technical problem to be solved in the present invention is to provide a kind of perfect heat-dissipating on graphical gallium nitride monocrystal substrate
The method for preparing gallium nitride light-emitting diode.
In order to solve the above-mentioned technical problem, the present invention takes following scheme：
A kind of method that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate, includes the following steps：
Step 1, the SiO that deposition thickness is 98-102nm on gallium nitride monocrystal substrate2Or SiN is as mask pattern layer,
The mask pattern layer is prepared as again the round poroid mask pattern layer with periodic structure, the round poroid mask pattern layer
Circular apertures it is 0.8-1.0 microns a diameter of, figure period of the round poroid mask pattern layer is 1.4-1.6 microns；
Step 2, it is anti-to be put into MOCVD after the gallium nitride monocrystal substrate that preparation has round poroid mask pattern layer being cleaned up
Room is answered to carry out diauxic growth, in H2Atmosphere, at 950-1050 DEG C, the pressure of MOCVD reative cells is rubbed for 200-300torr, V/III
, than being 1000-1300, three dimensional growth thickness is 150-200 nanometers of N-shaped GaN three dimensional growth layers for you；
Step 3, in H2Atmosphere, at 1050-1100 DEG C, the pressure of MOCVD reative cells is 60-100torr, V/III mole
Than for 1300-3000, the N-shaped GaN two dimensions that two-dimensional growth thickness is 1-3 microns merge layer；
Step 4, in N2Atmosphere, at 820-850 DEG C, V/III molar ratios are 5000-10000, the pressure of MOCVD reative cells
For 300torr, growth thickness is the N-shaped GaN low temperature stress release layers of 150nm；
Step 5, in N2Atmosphere, at 750-850 DEG C, V/III molar ratios are 5000-10000, the pressure of MOCVD reative cells
For 300torr, the In in 5-10 periods is grownxGa1-xN/GaN multi-quantum well active regions, wherein, 0<X≤0.3, InxGa1-xN well layer
Thickness range in 2-4nm, the thickness of GaN barrier layer is 8-20nm；
Step 6, in N2Atmosphere, at 850-950 DEG C, V/III molar ratios are the pressure of 5000-10000, MOCVD reative cell
For 100-300torr, the p-type Al in 5-10 period is growny1Ga1-y1N/GaN superlattices electronic barrier layers, wherein, Al components 0≤
y1≤ 0.2, p-type Aly1Ga1-y1The thickness of N is 2-5nm, and GaN layer thickness is 2-5nm；
Step 7, in H2Atmosphere, at 950-1050 DEG C, V/III molar ratios are the pressure of 2000-5000, MOCVD reative cell
For 100torr, the high temperature p-type GaN layer of 100-300nm is grown；
Step 8, in H2Atmosphere, at 650-750 DEG C, V/III molar ratios are the pressure of 5000-10000, MOCVD reative cell
For 300torr, the p-type InGaN contact layers of 2-4nm are grown；
Step 9, the temperature of MOCVD reative cells is down to 20-30 DEG C, terminates growth, completed outside gallium nitride light-emitting diode
Prolong the growth of layer, the GaN base light emitting epitaxial layer of high brightness is prepared.
Mask pattern layer is prepared using chemical vapor deposition manner in the step 1.
Three dimensional growth N-shaped GaN three dimensional growth layers, the n are carried out using the growth rate of micro- m/h of 1-3 in the step 2
The Si doping concentrations of type GaN three dimensional growth layers are 1018-1019cm-3。
Growing n-type GaN two dimensions are carried out using constant growth rate in the step 3 and merge layer, N-shaped GaN two dimensions merge
The Si doping concentrations of layer are 1018-1019cm-3。
P-type Al in the step 6y1Ga1-y1The corresponding hole concentration of Mg doping concentrations of N/GaN superlattices electronic barrier layers
It is 2 × 1017cm-3, wherein Al components reduce with the increase of number of superlattice cycles in superlattices electronic barrier layer.
Subtract when the Al components are reduced with the increase of number of superlattice cycles in superlattices electronic barrier layer in staged
It is few.
The Mg doping concentrations of high temperature p-type GaN layer in the step 7 are 1017-1018cm-3。
The Mg doping concentrations of p-type InGaN contact layers in the step 8 are more than 1018cm-3。
The temperature of MOCVD reative cells is first down to 700-750 DEG C in the step 9, is then carried out using pure nitrogen gas atmosphere
Annealing 5-20 minutes, then it is down to 20-30 DEG C.
The ginsengs such as carrier gas, growth temperature and growth rate of the present invention by optimizing gallium nitride monocrystal substrate early growth period
Number, controls the growth pattern of epitaxial layer of gallium nitride, prepares high-crystal quality epitaxial layer of gallium nitride, prepare height on this basis
The GaN base LED epitaxial layers of brightness have good heat dissipation performance.
Description of the drawings
Attached drawing 1 is the cross-sectional view of gallium nitride light-emitting diode that the method for the present invention is prepared.
Specific embodiment
For the ease of the understanding of those skilled in the art, the present invention is made in the following with reference to the drawings and specific embodiments further
Description.
The present invention is reacted using the vertical reative cell MOCVD growing systems of close coupling in Metal Organic Vapor extension
Diauxic growth is carried out in the MOCVD reative cells of room, completes the growth of gallium nitride light-emitting diode epitaxial layer, as shown in Figure 1, the nitrogen
The structure for changing gallium emitting diode epitaxial layer includes preparing GaN single crystal substrate 101, the n for having mask pattern layer from lower to upper successively
Type GaN three dimensional growths layer 102, N-shaped GaN two dimensions merge layer 103, n-type GaN layer low temperature stress release layer 104, InxGa1-xN/
GaN multi-quantum well active regions 105, p-type Aly1Ga1-y1N/GaN superlattices electronic barrier layer 106, high temperature p-type GaN layer 107 and p-type
InGaN contact layers 108.In the growth course of gallium nitride light-emitting diode epitaxial layer, with trimethyl gallium（TMGa）, triethyl-gallium
（TEGa）, trimethyl indium（TMIn）, trimethyl aluminium（TMAl）As group III source, ammonia（NH3）Respectively as Ga, Al, In and N
Source, with silane（SiH4）As n-type dopant, two luxuriant magnesium（Cp2Mg）As p-type dopant.
The specific preparation method of the present invention is described in detail with embodiment below.
Embodiment 1
A kind of method that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate, includes the following steps：
Step 1, using chemical vapor deposition manner（PECVD）Deposition thickness is 100nm's on gallium nitride monocrystal substrate
SiO2Or SiN is as mask pattern layer, then the round poroid mask figure that the mask pattern layer is prepared as having periodic structure
Shape layer, a diameter of 0.9 micron of the circular apertures of the round poroid mask pattern layer, the figure period of the round poroid mask pattern layer
It is 1.5 microns.
Step 2, it is put into after the gallium nitride monocrystal substrate 101 that preparation has round poroid mask pattern layer being cleaned up
MOCVD reative cells carry out diauxic growth, in H2Atmosphere, at 1000 DEG C, the pressure of MOCVD reative cells is rubbed for 250torr, V/III
You are than for 1200, using 1 micro- m/h of growth rate three dimensional growth thickness as 175 nanometers of N-shaped GaN three dimensional growth layers
102, the wherein Si doping concentrations of N-shaped GaN three dimensional growth layers are 1018cm-3。
Step 3, in H2Atmosphere, at 1075 DEG C, it is 2150 that the pressure of MOCVD reative cells, which is 80torr, V/III molar ratio,
Constant growth rate two-dimensional growth thickness is used to merge layer 103 for 2 microns of N-shaped GaN two dimensions；Wherein N-shaped GaN two dimensions merge
The Si doping concentrations of layer are 1018cm-3。
Step 4, in N2Atmosphere, at 830 DEG C, V/III molar ratios are that the pressure of 8000, MOCVD reative cells is 300torr,
Growth thickness is the N-shaped GaN low temperature stress release layer 104 of 150nm.
Step 5, in N2Atmosphere, at 800 DEG C, V/III molar ratios are that the pressure of 8000, MOCVD reative cells is 300torr,
Grow the In in 8 periodsxGa1-xN/GaN multi-quantum well active regions 105, wherein, x 0.1, InxGa1-xThe thickness range of N well layer is
The thickness of 2nm, GaN barrier layer is 8nm.
Step 6, in N2Atmosphere, at 900 DEG C, V/III molar ratios are 8000, the pressure of MOCVD reative cells is 200torr,
Grow the p-type Al in 8 periodsy1Ga1-y1N/GaN superlattices electronic barrier layer 106, wherein, Al components y1It is 0.1, the Al components
With the increase of number of superlattice cycles in superlattices electronic barrier layer, staged is reduced, p-type Aly1Ga1-y1The thickness of N is 2nm,
GaN layer thickness is 2nm, p-type Aly1Ga1-y1The corresponding hole concentration of Mg doping concentrations of N/GaN superlattices electronic barrier layers is 2
×1017cm-3。
Step 7, in H2Atmosphere, at 1000 DEG C, V/III molar ratios are 3500, the pressure of MOCVD reative cells is 100torr,
The high temperature p-type GaN layer 107 of 200nm is grown, the Mg doping concentrations of the high temperature p-type GaN layer are 1017cm-3。
Step 8, in H2Atmosphere, at 700 DEG C, V/III molar ratios are 8000, the pressure of MOCVD reative cells is 300torr,
The p-type InGaN contact layers 108 of 2nm are grown, the Mg doping concentrations of p-type InGaN contact layers are more than 1018cm-3。
Step 9, the temperature of MOCVD reative cells is first down to 700 DEG C, annealing 5 is then carried out using pure nitrogen gas atmosphere
Minute, then 20 DEG C are down to, terminate growth, complete the growth of gallium nitride light-emitting diode epitaxial layer, the GaN of high brightness is prepared
Based light-emitting diode epitaxial layer.
Embodiment two
Step 1, using chemical vapor deposition manner（PECVD）Deposition thickness is 98nm's on gallium nitride monocrystal substrate
SiO2Or SiN is as mask pattern layer, then the round poroid mask figure that the mask pattern layer is prepared as having periodic structure
Shape layer, a diameter of 0.8 micron of the circular apertures of the round poroid mask pattern layer, the figure period of the round poroid mask pattern layer
It is 1.4 microns.
Step 2, it is put into after the gallium nitride monocrystal substrate 101 that preparation has round poroid mask pattern layer being cleaned up
MOCVD reative cells carry out diauxic growth, in H2Atmosphere, at 950 DEG C, the pressure of MOCVD reative cells is 200torr, V/III mole
Than being 1000,2 micro- ms/h of growth rate three dimensional growth thickness is used as 150 nanometers of N-shaped GaN three dimensional growths layer 102,
Wherein the Si doping concentrations of N-shaped GaN three dimensional growth layers are 1019cm-3。
Step 3, in H2Atmosphere, at 1050 DEG C, it is 1300 that the pressure of MOCVD reative cells, which is 60torr, V/III molar ratio,
Constant growth rate two-dimensional growth thickness is used to merge layer 103 for 2 microns of N-shaped GaN two dimensions；Wherein N-shaped GaN two dimensions merge
The Si doping concentrations of layer are 1019cm-3。
Step 4, in N2Atmosphere, at 820 DEG C, V/III molar ratios are that the pressure of 5000, MOCVD reative cells is 300torr,
Growth thickness is the N-shaped GaN low temperature stress release layer 104 of 150nm.
Step 5, in N2Atmosphere, at 750 DEG C, V/III molar ratios are that the pressure of 5000, MOCVD reative cells is 300torr,
Grow the In in 5 periodsxGa1-xN/GaN multi-quantum well active regions 105, wherein, x 0.2, InxGa1-xThe thickness range of N well layer is
The thickness of 3nm, GaN barrier layer is 15nm.
Step 6, in N2Atmosphere, at 850 DEG C, V/III molar ratios are 5000, the pressure of MOCVD reative cells is 100torr,
Grow the p-type Al in 5 periodsy1Ga1-y1N/GaN superlattices electronic barrier layer 106, wherein, Al components y1Be 0, the Al components with
The increase of number of superlattice cycles in superlattices electronic barrier layer and staged is reduced, p-type Aly1Ga1-y1The thickness of N is 3nm,
GaN layer thickness is 4nm, p-type Aly1Ga1-y1The corresponding hole concentration of Mg doping concentrations of N/GaN superlattices electronic barrier layers is 2
×1017cm-3。
Step 7, in H2Atmosphere, at 950 DEG C, V/III molar ratios are 2000, the pressure of MOCVD reative cells is 100torr,
The high temperature p-type GaN layer 107 of 100nm is grown, the Mg doping concentrations of high temperature p-type GaN layer are 1018cm-3。
Step 8, in H2Atmosphere, at 650 DEG C, V/III molar ratios are 5000, the pressure of MOCVD reative cells is 300torr,
The p-type InGaN contact layers 108 of 3nm are grown, the Mg doping concentrations of p-type InGaN contact layers are more than 1018cm-3。
Step 9, the temperature of MOCVD reative cells is first down to 720 DEG C, annealing 10 is then carried out using pure nitrogen gas atmosphere
Minute, then 25 DEG C are down to, terminate growth, complete the growth of gallium nitride light-emitting diode epitaxial layer, the GaN of high brightness is prepared
Based light-emitting diode epitaxial layer.
Embodiment three
Step 1, using chemical vapor deposition manner（PECVD）Deposition thickness is 102nm's on gallium nitride monocrystal substrate
SiO2Or SiN is as mask pattern layer, then the round poroid mask figure that the mask pattern layer is prepared as having periodic structure
Shape layer, a diameter of 1.0 microns of the circular apertures of the round poroid mask pattern layer, the figure period of the round poroid mask pattern layer
It is 1.6 microns.
Step 2, it is put into after the gallium nitride monocrystal substrate 101 that preparation has round poroid mask pattern layer being cleaned up
MOCVD reative cells carry out diauxic growth, in H2Atmosphere, at 1050 DEG C, the pressure of MOCVD reative cells is rubbed for 300torr, V/III
You are than for 1300, using 3 micro- ms/h of growth rate three dimensional growth thickness as 200 nanometers of N-shaped GaN three dimensional growth layers
102, the wherein Si doping concentrations of N-shaped GaN three dimensional growth layers are 1019cm-3。
Step 3, in H2Atmosphere, at 1100 DEG C, it is 3000 that the pressure of MOCVD reative cells, which is 100torr, V/III molar ratio,
Constant growth rate two-dimensional growth thickness is used to merge layer 103 for 2 microns of N-shaped GaN two dimensions；Wherein N-shaped GaN two dimensions merge
The Si doping concentrations of layer are 1019cm-3。
Step 4, in N2Atmosphere, at 850 DEG C, V/III molar ratios are that the pressure of 10000, MOCVD reative cells is 300torr,
Growth thickness is the N-shaped GaN low temperature stress release layer 104 of 150nm.
Step 5, in N2Atmosphere, at 850 DEG C, V/III molar ratios are that the pressure of 10000, MOCVD reative cells is 300torr,
Grow the In in 10 periodsxGa1-xN/GaN multi-quantum well active regions 105, wherein, x 0.3, InxGa1-xThe thickness range of N well layer
For 4nm, the thickness of GaN barrier layer is 20nm.
Step 6, in N2Atmosphere, at 950 DEG C, V/III molar ratios are 10000, the pressure of MOCVD reative cells is 300torr,
Grow the p-type Al in 10 periodsy1Ga1-y1N/GaN superlattices electronic barrier layer 106, wherein, Al components y1It is 0.2, the Al components
With the increase of number of superlattice cycles in superlattices electronic barrier layer, staged is reduced, p-type Aly1Ga1-y1The thickness of N is 5nm,
GaN layer thickness is 5nm, p-type Aly1Ga1-y1The corresponding hole concentration of Mg doping concentrations of N/GaN superlattices electronic barrier layers is 2
×1017cm-3。
Step 7, in H2Atmosphere, at 1050 DEG C, V/III molar ratios are 5000, the pressure of MOCVD reative cells is 100torr,
The high temperature p-type GaN layer 107 of 300nm is grown, the Mg doping concentrations of the high temperature p-type GaN layer are 1018cm-3。
Step 8, in H2Atmosphere, at 750 DEG C, V/III molar ratios are 10000, the pressure of MOCVD reative cells is
300torr, grows the p-type InGaN contact layers 108 of 4nm, and the Mg doping concentrations of p-type InGaN contact layers are more than 1018cm-3。
Step 9, the temperature of MOCVD reative cells is first down to 750 DEG C, annealing 20 is then carried out using pure nitrogen gas atmosphere
Minute, then 30 DEG C are down to, terminate growth, complete the growth of gallium nitride light-emitting diode epitaxial layer, the GaN of high brightness is prepared
Based light-emitting diode epitaxial layer.
Embodiment described above is merely illustrative of the invention's technical idea and feature, and description is more specific and detailed,
Its object is to which those of ordinary skill in the art is enable to understand present disclosure and are implemented according to this, therefore cannot be only with this
Come limit the present invention scope of patent protection, can not therefore and be interpreted as limitation of the scope of the invention.It should be pointed out that
For those of ordinary skill in the art, without departing from the concept of the premise of the invention, several changes can also be made
Shape and improvement, i.e., the variation that all spirit revealed according to the present invention is made should cover the scope of patent protection in the present invention
It is interior.
Claims (9)
1. a kind of method that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate, includes the following steps：
Step 1, the SiO that deposition thickness is 98-102nm on gallium nitride monocrystal substrate2Or SiN is as mask pattern layer, then this
Mask pattern layer is prepared as the round poroid mask pattern layer with periodic structure, the round poroid mask pattern layer it is round
Bore dia is 0.8-1.0 microns, and the figure period of the round poroid mask pattern layer is 1.4-1.6 microns；
Step 2, MOCVD reative cells are put into after the gallium nitride monocrystal substrate that preparation has round poroid mask pattern layer being cleaned up
Diauxic growth is carried out, in H2Atmosphere, at 950-1050 DEG C, the pressure of MOCVD reative cells is 200-300torr, V/III molar ratio
For 1000-1300, three dimensional growth thickness is the N-shaped GaN three dimensional growth layers of 150-200 nm；
Step 3, in H2Atmosphere, at 1050-1100 DEG C, the pressure of MOCVD reative cells is that 60-100torr, V/III molar ratio are
1300-3000, the N-shaped GaN two dimensions that two-dimensional growth thickness is 1-3 microns merge layer；
Step 4, in N2Atmosphere, at 820-850 DEG C, V/III molar ratios are 5000-10000, and the pressure of MOCVD reative cells is
300torr, growth thickness are the N-shaped GaN low temperature stress release layers of 150nm；
Step 5, in N2Atmosphere, at 750-850 DEG C, V/III molar ratios are 5000-10000, and the pressure of MOCVD reative cells is
300torr grows the In in 5-10 periodsxGa1-xN/GaN multi-quantum well active regions, wherein, 0<X≤0.3, InxGa1-xN well layer
For thickness range in 2-4nm, the thickness of GaN barrier layer is 8-20nm；
Step 6, in N2Atmosphere, at 850-950 DEG C, V/III molar ratios are that the pressure of 5000-10000, MOCVD reative cell is 100-
300torr grows the p-type Al in 5-10 periody1Ga1-y1N/GaN superlattices electronic barrier layers, wherein, 0≤y of Al components1≤
0.2, p-type Aly1Ga1-y1The thickness of N is 2-5nm, and GaN layer thickness is 2-5nm；
Step 7, in H2Atmosphere, at 950-1050 DEG C, V/III molar ratios are that the pressure of 2000-5000, MOCVD reative cell is
100torr grows the high temperature p-type GaN layer of 100-300nm；
Step 8, in H2Atmosphere, at 650-750 DEG C, V/III molar ratios are that the pressure of 5000-10000, MOCVD reative cell is
300torr grows the p-type InGaN contact layers of 2-4nm；
Step 9, the temperature of MOCVD reative cells is down to 20-30 DEG C, terminates growth, complete gallium nitride light-emitting diode epitaxial layer
Growth, the GaN base light emitting epitaxial layer of high brightness is prepared.
2. the method according to claim 1 that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate,
It is characterized in that, mask pattern layer is prepared using chemical vapor deposition manner in the step 1.
3. the method according to claim 2 that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate,
It is characterized in that, three dimensional growth N-shaped GaN three dimensional growth layers are carried out using the growth rate of micro- m/h of 1-3 in the step 2,
The Si doping concentrations of N-shaped GaN three dimensional growth layers are 1018-1019cm-3。
4. the method according to claim 3 that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate,
It is characterized in that, carrying out growing n-type GaN two dimensions using constant growth rate in the step 3 merges layer, N-shaped GaN two dimensions are closed
And the Si doping concentrations of layer are 1018-1019cm-3。
5. the method according to claim 4 that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate,
It is characterized in that, p-type Al in the step 6y1Ga1-y1The corresponding hole of Mg doping concentrations of N/GaN superlattices electronic barrier layers
A concentration of 2 × 1017cm-3, wherein Al components reduce with the increase of number of superlattice cycles in superlattices electronic barrier layer.
6. the method according to claim 5 that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate,
It is characterized in that, it is in staged when the Al components are reduced with the increase of number of superlattice cycles in superlattices electronic barrier layer
It reduces.
7. the method according to claim 6 that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate,
It is characterized in that, the Mg doping concentrations of the high temperature p-type GaN layer in the step 7 are 1017-1018cm-3。
8. the method according to claim 7 that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate,
It is characterized in that, the Mg doping concentrations of the p-type InGaN contact layers in the step 8 are more than 1018cm-3。
9. the method according to claim 8 that gallium nitride light-emitting diode is prepared on graphical gallium nitride monocrystal substrate,
It is characterized in that, the temperature of MOCVD reative cells is first down to 700-750 DEG C in the step 9, then using pure nitrogen gas atmosphere into
Row annealing 5-20 minutes, then it is down to 20-30 DEG C.
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