CN106229389B - A kind of method that light emitting diode is prepared in nitride metal gallium compound substrate - Google Patents
A kind of method that light emitting diode is prepared in nitride metal gallium compound substrate Download PDFInfo
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- CN106229389B CN106229389B CN201610631817.8A CN201610631817A CN106229389B CN 106229389 B CN106229389 B CN 106229389B CN 201610631817 A CN201610631817 A CN 201610631817A CN 106229389 B CN106229389 B CN 106229389B
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- 239000000758 substrate Substances 0.000 title claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 44
- 239000002184 metal Substances 0.000 title claims abstract description 44
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 41
- 150000002259 gallium compounds Chemical class 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000004888 barrier function Effects 0.000 claims abstract description 59
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 27
- 239000012298 atmosphere Substances 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims description 61
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 abstract description 2
- 229910002601 GaN Inorganic materials 0.000 description 53
- 239000011777 magnesium Substances 0.000 description 23
- 230000035882 stress Effects 0.000 description 11
- 230000017525 heat dissipation Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910052733 gallium Inorganic materials 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 239000000463 material Substances 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
- 239000004593 Epoxy Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 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
- 239000002131 composite material 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
- 238000000407 epitaxy Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/04—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/12—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a stress relaxation structure, e.g. buffer layer
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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
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/14—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a carrier transport control structure, e.g. highly-doped semiconductor layer or current-blocking structure
- H01L33/145—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a carrier transport control structure, e.g. highly-doped semiconductor layer or current-blocking structure with a current-blocking structure
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Abstract
A kind of method that light emitting diode is prepared in nitride metal gallium compound substrate, includes the following steps, first in N2Atmosphere, 820 850 DEG C, under chamber pressure 300torr, epitaxial thickness is 200 nanometers of low temperature N-shaped GaN stress release layers in metal GaN compound substrates, then in N2Atmosphere at 750 850 DEG C, grows the In of multicyclexGa1‑xN/GaN multi-quantum well active regions；Then in H2Atmosphere at 850 95 DEG C, grows p-type Aly1Inx1Ga1‑y1‑x1N electronic barrier layers, then in H2Atmosphere at 950 1050 DEG C, grows high temperature p-type GaN layer；Then again in H2Atmosphere grows p-type InGaN contact layers at 650 750 DEG C, and high brightness nitride metal gallium compound substrate light emitting diode is prepared in annealing.The present invention improves nitride metal gallium compound substrate light-emitting diode luminous efficiency.
Description
Technical field
The present invention relates to field of semiconductor photoelectron technique, one kind prepares high brightness hair in nitride metal gallium compound substrate
The method of optical 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.And the thermal capacity very littles of LED in itself, institute
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
Amount 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 dissipate
Heat, 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, the about 25W/ at 100 °C（m-
K）.LED heat dissipation problems can effectively be solved using nitride metal gallium compound substrate, however, as metal substrate and epitaxy of gallium nitride
There are larger thermal mismatchings between layer, prepare the brightness people not to the utmost of light emitting diode in nitride metal gallium compound substrate at present
Meaning.
Invention content
The technical problem to be solved in the present invention is to provide a kind of thermal diffusivity is good, being answered in nitride metal gallium for luminous efficiency is improved
Close the method that light emitting diode is prepared on substrate.
In order to solve the above-mentioned technical problem, the present invention takes following scheme：
A kind of method that light emitting diode is prepared in nitride metal gallium compound substrate, includes the following steps：
Step 1, nitride metal gallium compound substrate is put into MOCVD reative cells, in N2Atmosphere, MOCVD chamber pressures
Under 300torr, MOCVD reative cells to be warming up to 820-850 DEG C, are then made annealing treatment within the temperature range of 820-850 DEG C
55~65s, then using MOCVD chamber pressure 300torr, V/III molar ratios as 500-1300, using 0.2 micro- m/h -1
Micro- m/h of growth rate, growth thickness are 200 nanometers of low temperature N-shaped GaN stress release layers；
Step 2, in N2Atmosphere, at 750-850 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressures
For 300torr, the In in 3-10 period is grownxGa1-xN/GaN multi-quantum well active regions, wherein, 0<x≤0.3；
Step 3, in N2Atmosphere, at 850-950 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressure
For 100-300torr, growth thickness is 30 nanometers of p-type Aly1Inx1Ga1-y1-x1N electronic barrier layers, 0≤y of Al components1≤
0.2, In 0≤x of component1≤x；
Step 4, in H2Atmosphere, at 950-1050 DEG C, using V/III molar ratios as 2000-5000, MOCVD chamber pressure
For 100torr, growth thickness is the high temperature p-type GaN layer of 100-300nm；
Step 5, in H2Atmosphere, at 650-750 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressure
For 300torr, growth thickness is the p-type InGaN contact layers of 2-4nm；
Step 6, the temperature of MOCVD reative cells is down to 20-30 DEG C, terminates growth, complete nitride metal gallium compound substrate
The nitride metal gallium compound substrate light emitting diode of high brightness is prepared in the growth of emitting diode epitaxial layer.
The Si doping concentrations of low temperature N-shaped GaN stress release layers are 10 in the step 118-1019cm-3。
In is grown in the step 2xGa1-xN/GaN multi-quantum well active regions specifically include：
Step 2.1, in N2Atmosphere, at 750-850 DEG C, using V/III molar ratios as 5000-10000, MOCVD reaction chamber pressures
Power is 300torr, first grows the In in 3 periodsxGa1-xN/GaN multi-quantum well active regions, wherein, 0<X≤0.3, InxGa1-xN traps
It is 8-20nm that the thickness of layer, which is 2-4nm, GaN barrier layer thickness, and wherein the Si doping concentrations of GaN barrier layer are 1017cm-3；
Step 2.2, then it is further continued for the In in 7 periods of growthxGa1-xN/GaN multi-quantum well active regions, wherein, 0<x≤
0.3, InxGa1-xThe thickness of N well layer is that 2-4nm, GaN barrier layer thickness are 8-20nm, and wherein GaN barrier layer mixes layer to be non-.
P-type Al is grown in the step 3y1Inx1Ga1-y1-x1N electronic barrier layers specifically include：
Step 3.1, in N2Atmosphere at 850-950 DEG C, reacts chamber pressure by 5000-10000, MOCVD of V/III molar ratios
Power is 100-300torr, and first growth thickness is 30 nanometers of p-type Aly1Inx1Ga1-y1-x1N electronic barrier layers, the p-type
Aly1Inx1Ga1-y1-x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 1 × 1017cm-3, wherein, Al components 0≤
y10≤x of≤0.2, In component1≤x；
Step 3.2, then it is further continued for the p-type Al that growth thickness is 30 nanometersy1Inx1Ga1-y1-x1N electronic barrier layers, the p-type
Aly1Inx1Ga1-y1-x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 2 × 1017cm-3, wherein, Al components 0≤
y10≤x of≤0.2, In component1≤x。
The Mg doping concentrations of high temperature p-type GaN layer in the step 4 are 5 × 1017cm-3。
P-type InGaN contact layer Mg doping concentrations in the step 5 are more than 1018cm-3。
The step 6 is specially that the temperature of MOCVD reative cells is first down to 700-750 DEG C, then using pure nitrogen gas atmosphere
It carries out annealing 5-20 minutes, then is down to 20-30 DEG C.
The present invention by the extension low temperature stress release layer between nitride metal gallium compound substrate and multi-quantum well active region,
Effectively alleviate active area compression, improve active area crystal quality.Quantum barrier layer is adulterated by using Si stageds and Mg mixes
The electronic barrier layer of miscellaneous concentration step variation is effectively improved distribution of the electron hole in active area, improves nitride metal gallium and answers
Close substrate LED luminous efficiency.
Description of the drawings
The cross-sectional view for the light emitting diode that attached drawing 1 is prepared for the method for the present invention.
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
It is grown in the MOCVD reative cells of room, completes the growth of the emitting diode epitaxial layer in nitride metal gallium compound substrate.It is such as attached
Shown in Fig. 1, the structure of the emitting diode epitaxial layer is followed successively by nitride metal gallium compound substrate 101, low temperature N-shaped from lower to upper
GaN stress release layers 102, InxGa1-xN/GaN multi-quantum well active regions 103, p-type Aly1Inx1Ga1-y1-x1N electronic barrier layers
104th, high temperature p-type GaN layer 105, p-type InGaN contact layers 106.In growth course, 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.
With specific embodiment, the invention will be further elaborated below.
Embodiment one
A kind of method that light emitting diode is prepared in nitride metal gallium compound substrate, includes the following steps：
Step 1, nitride metal gallium compound substrate 101 is put into MOCVD reative cells, in N2Atmosphere, MOCVD reaction chamber pressures
Power is under 300torr, and MOCVD reative cells are warming up to 820 DEG C, then keeps being made annealing treatment under 820 DEG C of temperature conditions
55 seconds, then using MOCVD chamber pressure 300torr, V/III molar ratios as 500, using 0.2 micro- m/h of growth speed
Rate, growth thickness are 200 nanometers of low temperature N-shaped GaN stress release layers 102, and the Si doping of low temperature N-shaped GaN stress release layers is dense
Spend is 1018cm-3。
Step 2, in N2Atmosphere, at 750-850 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressures
For 300torr, the In in 3-10 period is grownxGa1-xN/GaN multi-quantum well active regions 103, wherein, 0<x≤0.3.
The step 2 specifically includes：Step 2.1, in N2Atmosphere, at 750 DEG C, it is anti-as 5000, MOCVD using V/III molar ratios
Chamber pressure is answered first to grow the In in 3 periods for 300torrxGa1-xN/GaN multi-quantum well active regions, wherein, x 0.1,
InxGa1-xThe thickness of N well layer is that 2nm, GaN barrier layer thickness are 8nm, and wherein the Si doping concentrations of GaN barrier layer are 1017cm-3。Gt
vb
Step 2.2, the N in step 2.1 is then kept2Atmosphere, at 750 DEG C, it is anti-as 5000, MOCVD using V/III molar ratios
Answer In of the chamber pressure to be further continued for 7 periods of growth in the case of 300torrxGa1-xN/GaN multi-quantum well active regions, wherein,
X is 0.1, InxGa1-xThe thickness of N well layer is that 2nm, GaN barrier layer thickness are 8nm, and wherein GaN barrier layer mixes layer to be non-.By above-mentioned
Growth, so as to obtain the doping concentration of barrier layer Si be in step variation InxGa1-xN/GaN multi-quantum well active regions.
Step 3, in N2Atmosphere, at 850-950 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressure
For 100-300torr, growth thickness is 30 nanometers of p-type Aly1Inx1Ga1-y1-x1N electronic barrier layers（104）, 0≤y of Al components1
0≤x of≤0.2, In component1≤x。
The step 3 specifically includes：Step 3.1, in N2Atmosphere, at 850 DEG C, it is anti-as 5000, MOCVD using V/III molar ratios
Chamber pressure is answered as 100torr, first growth thickness is 30 nanometers of p-type Aly1Inx1Ga1-y1-x1N electronic barrier layers, the p-type
Aly1Inx1Ga1-y1-x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 1 × 1017cm-3, wherein, Al components y1
For 0, In components x1It is 0.
Step 3.2, the N in step 3.1 is then kept2Atmosphere, at 850 DEG C, it is anti-as 5000, MOCVD using V/III molar ratios
The p-type Al that growth thickness is 30 nanometers is further continued in the case that answer chamber pressure be 100torry1Inx1Ga1-y1-x1N electronic barrier layers,
P-type Aly1Inx1Ga1-y1-x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 2 × 1017cm-3, wherein, Al groups
Divide y1For 0, In components x1It is 0.By above-mentioned growth, the p-type Al that Mg doping concentrations are in step variation is obtainedy1Inx1Ga1-y1- x1N electronic barrier layers.
Step 4, in H2Atmosphere, at 950 DEG C, using V/III molar ratios be 2000, MOCVD chamber pressures is 100torr,
Growth thickness is the high temperature p-type GaN layer 105 of 100nm, and the Mg doping concentrations of the high temperature p-type GaN layer are 5 × 1017cm-3。
Step 5, in H2Atmosphere, at 650 DEG C, using V/III molar ratios be 5000, MOCVD chamber pressures is 300torr,
Growth thickness is the p-type InGaN contact layers 106 of 2nm, and p-type InGaN contact layer Mg doping concentrations are more than 1018cm-3。
Step 6, 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, the growth of nitride metal gallium compound substrate emitting diode epitaxial layer is completed, high brightness is prepared
Nitride metal gallium compound substrate light emitting diode.
Embodiment two
A kind of method that light emitting diode is prepared in nitride metal gallium compound substrate, includes the following steps：
Step 1, nitride metal gallium compound substrate 101 is put into MOCVD reative cells, in N2Atmosphere, MOCVD reaction chamber pressures
Power is under 300torr, and MOCVD reative cells are warming up to 835 DEG C, then keeps being made annealing treatment under 835 DEG C of temperature conditions
60 seconds, then using MOCVD chamber pressure 300torr, V/III molar ratios as 900, using 0.6 micro- m/h of growth speed
Rate, growth thickness are 200 nanometers of low temperature N-shaped GaN stress release layers 102, and the Si doping of low temperature N-shaped GaN stress release layers is dense
Spend is 1019cm-3。
Step 2, in N2Atmosphere, at 750-850 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressures
For 300torr, the In in 3-10 period is grownxGa1-xN/GaN multi-quantum well active regions 103, wherein, 0<x≤0.3.
The step 2 specifically includes：Step 2.1, in N2Atmosphere, at 800 DEG C, it is anti-as 8000, MOCVD using V/III molar ratios
Chamber pressure is answered first to grow the In in 3 periods for 300torrxGa1-xN/GaN multi-quantum well active regions, wherein, x 0.2,
InxGa1-xThe thickness of N well layer is that 3nm, GaN barrier layer thickness are 14nm, and wherein the Si doping concentrations of GaN barrier layer are 1017cm-3。
Step 2.2, then it is further continued for the In in 7 periods of growthxGa1-xN/GaN multi-quantum well active regions, wherein, x is
0.2, InxGa1-xThe thickness of N well layer is that 3nm, GaN barrier layer thickness are 14nm, and wherein GaN barrier layer mixes layer to be non-.By above-mentioned
Growth, so as to obtain the In that the doping concentration of barrier layer Si is in step variationxGa1-xN/GaN multi-quantum well active regions.
Step 3, in N2Atmosphere, at 850-950 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressure
For 100-300torr, growth thickness is 30 nanometers of p-type Aly1Inx1Ga1-y1-x1N electronic barrier layers（104）, 0≤y of Al components1
0≤x of≤0.2, In component1≤x。
The step 3 specifically includes：Step 3.1, in N2Atmosphere, at 900 DEG C, it is anti-as 8000, MOCVD using V/III molar ratios
Chamber pressure is answered as 200torr, first growth thickness is 30 nanometers of p-type Aly1Inx1Ga1-y1-x1N electronic barrier layers, the p-type
Aly1Inx1Ga1-y1-x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 1 × 1017cm-3, wherein, Al components y1
For 0.1, In components x1It is 0.1.
Step 3.2, then it is further continued for the p-type Al that growth thickness is 30 nanometersy1Inx1Ga1-y1-x1N electronic barrier layers, the p-type
Aly1Inx1Ga1-y1-x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 2 × 1017cm-3, wherein, Al components y1
For 0.1, In components x1It is 0.1.By above-mentioned growth, the p-type Al that Mg doping concentrations are in step variation is obtainedy1Inx1Ga1-y1- x1N electronic barrier layers.
Step 4, in H2Atmosphere, at 1000 DEG C, using V/III molar ratios be 3500, MOCVD chamber pressures is 100torr,
Growth thickness is the high temperature p-type GaN layer 105 of 200nm, and the Mg doping concentrations of the high temperature p-type GaN layer are 5 × 1017cm-3。
Step 5, in H2Atmosphere, at 700 DEG C, using V/III molar ratios be 8000, MOCVD chamber pressures is 300torr,
Growth thickness is the p-type InGaN contact layers 106 of 3nm, and p-type InGaN contact layer Mg doping concentrations are more than 1018cm-3。
Step 6, 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, the growth of nitride metal gallium compound substrate emitting diode epitaxial layer is completed, high brightness is prepared
Nitride metal gallium compound substrate light emitting diode.
Embodiment three
A kind of method that light emitting diode is prepared in nitride metal gallium compound substrate, includes the following steps：
Step 1, nitride metal gallium compound substrate 101 is put into MOCVD reative cells, in N2Atmosphere, MOCVD reaction chamber pressures
Power is under 300torr, and MOCVD reative cells are warming up to 850 DEG C, then keeps being made annealing treatment under 850 DEG C of temperature conditions
65 seconds, then using MOCVD chamber pressure 300torr, V/III molar ratios as 1300, using 1.0 micro- ms/h of growth speed
Rate, growth thickness are 200 nanometers of low temperature N-shaped GaN stress release layers 102, and the Si doping of low temperature N-shaped GaN stress release layers is dense
Spend is 1019cm-3。
Step 2, in N2Atmosphere, at 750-850 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressures
For 300torr, the In in 3-10 period is grownxGa1-xN/GaN multi-quantum well active regions 103, wherein, 0<x≤0.3.
The step 2 specifically includes：Step 2.1, in N2Atmosphere, at 850 DEG C, it is anti-as 10000, MOCVD using V/III molar ratios
Chamber pressure is answered first to grow the In in 3 periods for 300torrxGa1-xN/GaN multi-quantum well active regions, wherein, x 0.3,
InxGa1-xThe thickness of N well layer is that 4nm, GaN barrier layer thickness are 20nm, and wherein the Si doping concentrations of GaN barrier layer are 1017cm-3。
Step 2.2, then it is further continued for the In in 7 periods of growthxGa1-xN/GaN multi-quantum well active regions, wherein, x is
0.3, InxGa1-xThe thickness of N well layer is that 4nm, GaN barrier layer thickness are 20nm, and wherein GaN barrier layer mixes layer to be non-.By above-mentioned
Growth, so as to obtain the In that the doping concentration of quantum barrier layer Si is in step variationxGa1-xN/GaN multi-quantum well active regions.
Step 3, in N2Atmosphere, at 850-950 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressure
For 100-300torr, growth thickness is 30 nanometers of p-type Aly1Inx1Ga1-y1-x1N electronic barrier layers（104）, 0≤y of Al components1
0≤x of≤0.2, In component1≤x。
The step 3 specifically includes：Step 3.1, in N2Atmosphere, at 950 DEG C, it is anti-as 10000, MOCVD using V/III molar ratios
Chamber pressure is answered as 300torr, first growth thickness is 30 nanometers of p-type Aly1Inx1Ga1-y1-x1N electronic barrier layers, the p-type
Aly1Inx1Ga1-y1-x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 1 × 1017cm-3, wherein, Al components y1
For 0.2, In components x1It is 0.3.
Step 3.2, then it is further continued for the p-type Al that growth thickness is 30 nanometersy1Inx1Ga1-y1-x1N electronic barrier layers, the p-type
Aly1Inx1Ga1-y1-x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 2 × 1017cm-3, wherein, Al components y1
For 0.2, In components x1It is 0.3.By above-mentioned growth, the p-type Al that Mg doping concentrations are in step variation is obtainedy1Inx1Ga1-y1- x1N electronic barrier layers.
Step 4, in H2Atmosphere, at 1050 DEG C, using V/III molar ratios be 5000, MOCVD chamber pressures is 100torr,
Growth thickness is the high temperature p-type GaN layer 105 of 300nm, and the Mg doping concentrations of the high temperature p-type GaN layer are 5 × 1017cm-3。
Step 5, in H2Atmosphere, at 750 DEG C, using V/III molar ratios be 10000, MOCVD chamber pressures is 300torr,
Growth thickness is the p-type InGaN contact layers 106 of 4nm, and p-type InGaN contact layer Mg doping concentrations are more than 1018cm-3。
Step 6, 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, the growth of nitride metal gallium compound substrate emitting diode epitaxial layer is completed, high brightness is prepared
Nitride metal gallium compound substrate light emitting diode.
The present invention by the extension low temperature stress release layer between nitride metal gallium compound substrate and multi-quantum well active region,
Effectively alleviate active area compression, improve active area crystal quality.Doping concentration by the quantum barrier layer Si for growing the multicycle
In the In of step variationxGa1-xN/GaN multi-quantum well active regions and Mg doping concentrations are in the p-type of step variation
Aly1Inx1Ga1-y1-x1N electronic barrier layers are effectively improved distribution of the electron hole in active area, improve nitride metal gallium composite lining
Bottom light-emitting diode luminous efficiency.
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 (7)
1. a kind of method that light emitting diode is prepared in nitride metal gallium compound substrate, includes the following steps：
Step 1, by nitride metal gallium compound substrate（101）It is put into MOCVD reative cells, in N2Atmosphere, MOCVD chamber pressures
Under 300torr, MOCVD reative cells to be warming up to 820-850 DEG C, are then made annealing treatment within the temperature range of 820-850 DEG C
55~65s, then using MOCVD chamber pressure 300torr, V/III molar ratios as 500-1300, using 0.2 micro- m/h -1
Micro- m/h of growth rate, growth thickness are the low temperature N-shaped GaN stress release layers of 200nm（102）；
Step 2, in N2Atmosphere, at 750-850 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressures are
300torr grows the In in 3-10 periodxGa1-xN/GaN multi-quantum well active regions（103）, wherein, 0<x≤0.3；
Step 3, in N2Atmosphere is 100- by 5000-10000, MOCVD chamber pressure of V/III molar ratios at 850-950 DEG C
300torr, growth thickness are the p-type Al of 30nmy1Inx1Ga1-y1-x1N electronic barrier layers（104）, 0≤y of Al components1≤ 0.2, In
0≤x of component1≤x；
Step 4, in H2Atmosphere at 950-1050 DEG C, is by 2000-5000, MOCVD chamber pressure of V/III molar ratios
100torr, growth thickness are the high temperature p-type GaN layer of 100-300nm（105）；
Step 5, in H2Atmosphere at 650-750 DEG C, is by 5000-10000, MOCVD chamber pressure of V/III molar ratios
300torr, growth thickness are the p-type InGaN contact layers of 2-4nm（106）；
Step 6, the temperature of MOCVD reative cells is down to 20-30 DEG C, terminates growth, completed nitride metal gallium compound substrate and shine
The nitride metal gallium compound substrate light emitting diode of high brightness is prepared in the growth of diode epitaxial layer.
2. the method according to claim 1 that light emitting diode is prepared in nitride metal gallium compound substrate, feature exist
In the Si doping concentrations of low temperature N-shaped GaN stress release layers are 10 in the step 118-1019cm-3。
3. the method according to claim 2 that light emitting diode is prepared in nitride metal gallium compound substrate, feature exist
In growing In in the step 2xGa1-xN/GaN multi-quantum well active regions specifically include：
Step 2.1, in N2Atmosphere, at 750-850 DEG C, using V/III molar ratios as 5000-10000, MOCVD chamber pressures are
300torr first grows the In in 3 periodsxGa1-xN/GaN multi-quantum well active regions, wherein, 0<X≤0.3, InxGa1-xN well layer
Thickness is that 2-4nm, GaN barrier layer thickness are 8-20nm, and wherein the Si doping concentrations of GaN barrier layer are 1017cm-3；
Step 2.2, then it is further continued for the In in 7 periods of growthxGa1-xN/GaN multi-quantum well active regions, wherein, 0<X≤0.3,
InxGa1-xThe thickness of N well layer is that 2-4nm, GaN barrier layer thickness are 8-20nm, and wherein GaN barrier layer mixes layer to be non-.
4. the method according to claim 3 that light emitting diode is prepared in nitride metal gallium compound substrate, feature exist
In growth p-type Al in the step 3y1Inx1Ga1-y1-x1N electronic barrier layers specifically include：
Step 3.1, in N2Atmosphere at 850-950 DEG C, is by 5000-10000, MOCVD chamber pressure of V/III molar ratios
100-300torr, first growth thickness are the p-type Al of 30nmy1Inx1Ga1-y1-x1N electronic barrier layers, p-type Aly1Inx1Ga1-y1- x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 1 × 1017cm-3, wherein, 0≤y of Al components1≤ 0.2, In group
Divide 0≤x1≤x；
Step 3.2, then it is further continued for the p-type Al that growth thickness is 30nmy1Inx1Ga1-y1-x1N electronic barrier layers, the p-type
Aly1Inx1Ga1-y1-x1The corresponding hole concentration of Mg doping concentrations of N electronic barrier layers is 2 × 1017cm-3, wherein, Al components 0≤
y10≤x of≤0.2, In component1≤x。
5. the method according to claim 4 that light emitting diode is prepared in nitride metal gallium compound substrate, feature exist
In the Mg doping concentrations of the high temperature p-type GaN layer in the step 4 are 5 × 1017cm-3。
6. the method according to claim 5 that light emitting diode is prepared in nitride metal gallium compound substrate, feature exist
In the p-type InGaN contact layer Mg doping concentrations in the step 5 are more than 1018cm-3。
7. the method according to claim 6 that light emitting diode is prepared in nitride metal gallium compound substrate, feature exist
In the step 6 is specially that the temperature of MOCVD reative cells is first down to 700-750 DEG C, is then moved back using pure nitrogen gas atmosphere
Fire processing 5-20 minutes, then it is down to 20-30 DEG C.
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| CN110739374B (en) * | 2019-10-25 | 2021-01-26 | 圆融光电科技股份有限公司 | Growth method of electron blocking layer in light emitting diode and light emitting diode |
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| CN103305908A (en) * | 2012-03-14 | 2013-09-18 | 东莞市中镓半导体科技有限公司 | Composite substrate for GaN growth |
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