CN105742416B - A kind of preparation method of high-luminous-efficiency GaN-based LED epitaxial wafer - Google Patents
A kind of preparation method of high-luminous-efficiency GaN-based LED epitaxial wafer Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 29
- 230000004888 barrier function Effects 0.000 claims abstract description 25
- 230000026267 regulation of growth Effects 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 49
- 239000000758 substrate Substances 0.000 claims description 28
- 229910052594 sapphire Inorganic materials 0.000 claims description 21
- 239000010980 sapphire Substances 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 238000005530 etching Methods 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000011800 void material Substances 0.000 claims description 9
- 229910002704 AlGaN Inorganic materials 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 2
- 235000001674 Agaricus brunnescens Nutrition 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 4
- 230000005693 optoelectronics Effects 0.000 abstract description 2
- 229910002601 GaN Inorganic materials 0.000 description 190
- 238000010586 diagram Methods 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 8
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 7
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 230000006911 nucleation Effects 0.000 description 5
- 238000010899 nucleation Methods 0.000 description 5
- 238000001259 photo etching Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000001312 dry etching Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000004038 photonic crystal Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound 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
- 238000001039 wet etching Methods 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
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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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
- H01L33/20—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 particular shape, e.g. curved or truncated substrate
- H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers
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Abstract
The invention belongs to field of optoelectronic devices, and in particular to a kind of preparation method of high-luminous-efficiency GaN-based LED epitaxial wafer.The structure that this method is made includes low temperature GaN nucleating layers, the GaN rough layers of engraved structure, undoped GaN layer, N-type GaN layer, multiple quantum well active layer, electronic barrier layer and the p-type GaN layer stacked gradually.The GaN rough layers of wherein growth engraved structure include the 3D structure GaNs layer of first growth the first, then use H2Gas is handled the first 3D structure GaNs layer at high temperature, then the 3D structure GaNs layer of growth regulation two, finally grows the quick merging layer of 3D structure GaNs layer so that distribution is produced in the merging process on Dao Yu islands than more uniform cavity.The present invention uses H2Handle 3D structure GaNs layer, the GaN island structures of acquisition in size and spatial distribution all evenly, so that the cavity produced in the quick merging process of 3D structure GaNs layer is also evenly, the GaN rough layers of this engraved structure can reduce total internal reflection, be conducive to improving GaN base LED light extraction efficiency.
Description
Technical field
The invention belongs to field of optoelectronic devices, and in particular to a kind of system of high-luminous-efficiency GaN-based LED epitaxial wafer
Preparation Method.
Background technology
Gallium nitride based light emitting diode（Light Emitting Diode, LED）With high brightness, low energy consumption, the long-life,
The features such as fast response time and environmental protection, it is widely used in indoor and street lighting, traffic signals and outdoor display, Automobile
The multiple fields such as lamp illumination, liquid crystal backlight.Therefore, large power white light LED is considered as the lighting source of 21 century.
In order to obtain the LED of high brightness, it is critical to the internal quantum efficiency and external quantum efficiency for improving device.Current blue light
The LED internal quantum efficiency of GaN bases is up to more than 80%, but the external quantum efficiency generally only 40% of high-power LED chip is left
It is right.The principal element that restriction external quantum efficiency is improved is that the light extraction efficiency of chip is relatively low, because the refraction of GaN materials
Rate (n=2.5) differs larger with the refractive index (n=1) of air and the refractive index (n=1.75) of Sapphire Substrate, causes air
The critical angle being totally reflected with GaN interfaces and sapphire with GaN interfaces only has 23.6 ° and 44.4 ° respectively, and active area is produced
Light only have minority to escape out body material.In order to improve the light extraction efficiency of chip, the main skill used both at home and abroad at present
Art scheme has growth distribution bragg reflection layer (DBR) structure, patterned substrate（PSS）Technology, surface texture technology and light
Sub- crystal technology etc..PSS requires very high to the rule degree of figure, and Sapphire Substrate is harder in addition, either dry etching
Or wet-etching technology, there is certain difficulty in the uniformity and uniformity of full wafer figure, and manufacturing process is to equipment
It is very high with technological requirement, cause high expensive.DBR and photonic crystal manufacture craft is relative complex, cost is higher, and surface coarsening
Technology uses dry etching or wet corrosion technique, and there is also very big challenge.
The content of the invention
It is an object of the invention to for drawbacks described above present in prior art, there is provided a kind of high-luminous-efficiency gallium nitride
The preparation method of base LED epitaxial wafer, and this method is simple, prepares cost relatively low.
The present invention adopts the following technical scheme that realization：A kind of system of high-luminous-efficiency GaN-based LED epitaxial wafer
Preparation Method, comprises the following steps：
Step one：Sapphire Substrate is subjected to cleaning substrate surface in reaction chamber atmosphere of hydrogen, reaction cavity temperature is
1060-1100 DEG C, the time is 5min-10min；
Step 2：Reaction chamber temperature is reduced to 520-550 DEG C, then in clean Grown on Sapphire Substrates low temperature
GaN nucleating layers, nucleating layer thickness is 20-40nm, and growth pressure is 400-700Torr；
Step 3：Reaction chamber temperature is increased to 950-1000 DEG C, and stable 2min, the high temperature for carrying out GaN nucleating layers is moved back
Fire, is passed through NH during this3Gas is to prevent GaN nucleating layers from decomposing completely.Then pass to metal organic source TMGa, GaN into
Stratum nucleare surface starts the GaN layer of the 3D structures of growth regulation one, and growth thickness is 200-300nm, and growth pressure is 400-700Torr,
The GaN layer of first 3D structures includes little GaN islands and great GaN islands；
Step 4：Reaction chamber temperature is increased in 1030-1110 DEG C, temperature-rise period and is passed through NH3Gas is to prevent first
The GaN layer of 3D structures is decomposed, and heating closes NH after terminating3Gas is passed through, and is only passed through H2Gas is carried out to the GaN of 3D structures
5-10min is handled, in the process H2Gas can be performed etching to the GaN layer of the first 3D structures, and little GaN islands can be etched
Fall, great GaN islands are then remained, little GaN islands and great GaN islands do not have clear and definite size to define, simply in etching process
Middle size little GaN islands are easily etched away, therefore the GaN islands being etched away are little GaN islands, and the GaN islands remained are
Big GaN islands；
Step 5：Reaction chamber temperature is reduced to 950-1000 DEG C, NH is passed through3Gas and metal organic source TMGa, in H2Gas
The GaN layer 500-1000nm of the 3D structures of continued growth the 2nd in the GaN layer of 3D structures after body processing, growth pressure is 400-
700Torr, the 3D structure GaNs layer expanded；
Step 6：Reaction chamber temperature is increased to 1050-1200 DEG C, mushroomed out in the GaN layer of the 3D structures of expansion
Undoped with GaN so that 3D island structures heal rapidly, and ultimately form interior void than more uniform the flat hollow out in surface
The GaN rough layers of structure, growth thickness is 1 ~ 2um, and growth pressure is 50-300Torr；
Step 7：The GaN layer of unintentional doping is grown, thickness is 1 ~ 2um, and growth temperature is 1050-1200 DEG C, growth pressure
Power is 50-300Torr；
Step 8：The GaN layer of Si doping is grown, this layer of carrier concentration is 1018-1019cm-3, thickness is 1-3um, raw
Long temperature is 1050-1200 DEG C, and growth pressure is 50-300Torr；
Step 9：The multiple quantum well active layer in 3-6 cycle is grown, wherein barrier layer is GaN, and well layer is InGaN, In
Component is calculated as 10-30% with mass fraction, and well layer thickness is 2-5nm, and temperature is 700-800 DEG C, and barrier layer thickness is 8-
13nm, growth temperature is 800-950 DEG C, and pressure is 200-500Torr in growth course；
Step 10：Al components in the thick p-AlGaN electronic barrier layers of 20-50nm, the layer are grown to be calculated as with mass fraction
10-20%, hole concentration is 1017-1018cm-3, growth temperature is 850 DEG C -1000 DEG C, and pressure is 50-300Torr；
Step 11：The GaN layer of Mg doping is grown, thickness is 100-300nm, and growth temperature is 850-1000 DEG C, growth
Pressure is 100-500Torr, and hole concentration is 1017-1018cm-3；
Step 12：After epitaxial growth terminates, the temperature of reaction chamber is down to 650-800 DEG C, entered in nitrogen atmosphere
Row annealing 5-15min, is then down to room temperature, terminates growth, obtain epitaxial wafer.
Epitaxial process of the present invention is in metal organic chemical vapor deposition technique（MOCVD）MOCVD reaction
Carried out in chamber, the order of LED epitaxial structures from bottom to top includes Sapphire Substrate, low temperature GaN nucleating layers, engraved structure successively
GaN rough layers, undoped GaN layer, N-type GaN layer, multiple quantum well active layer, electronic barrier layer and p-type GaN layer, the present invention is outer
With trimethyl gallium during epitaxial growth（TMGa）, triethyl-gallium（TEGa）, trimethyl aluminium（TMAl）, trimethyl indium（TMIn）
And ammonia（NH3）Respectively Ga, Al, In and N source, silane（SiH4）With two luxuriant magnesium（CP2Mg）For N, P type dopant.
The present invention grown by process above, on a sapphire substrate interior void than more uniform the flat hollow out in surface
Structure GaN rough layer, the GaN rough layers of the engraved structure can reduce total internal reflection, be conducive to the light for improving GaN base LED to carry
Take efficiency.In addition using the GaN 3D structure growth techniques of two steps, help to change the direction of growth of dislocation so that active area
Dislocation density is reduced, and improves the crystal mass of epitaxial wafer.
Brief description of the drawings
Fig. 1 is the flow chart that prior art grows epitaxial wafer, and it stacks gradually growing low temperature GaN on a sapphire substrate
Nucleating layer, undoped GaN, N-type GaN, multiple quantum well active layer, electronic barrier layer, p-type GaN layer.
Fig. 2 for the present invention growth epitaxial wafer flow chart, its stack gradually on a sapphire substrate growing low temperature GaN into
Stratum nucleare, the GaN layers of the first 3D structures, the GaN layers of the 2nd 3D structures, the quick merging layer of the GaN layers of 3D structures, undoped
GaN, N-type GaN, multiple quantum well active layer, electronic barrier layer, p-type GaN layer.
Fig. 3 is the schematic diagram after the GaN layers of the 3D structures of growth regulation one on epitaxial wafer.
Fig. 4 is H2Schematic diagram after the GaN layers of the 3D structures of high-temperature process the first.
Fig. 5 is the schematic diagram after the GaN layers of the 2nd 3D structures of growth.
The empty schematic diagram that Fig. 6 is internally formed after quickly merging for the GaN layers of 3D structures.
Fig. 7 is is respectively adopted made by the epitaxial wafer that epitaxial wafer and the commonsense method of the method growth that the present invention is provided grow
LED chip optical output power profiles versus figure.
Embodiment
Embodiment one：
A kind of preparation method of high-luminous-efficiency GaN-based LED epitaxial wafer, comprises the following steps：
Step one：Sapphire Substrate is carried out to temperature in cleaning substrate surface, reaction chamber in MOCVD reaction chamber atmosphere of hydrogen
Spend for 1060 DEG C, the time is 10min；
Step 2：Reaction chamber temperature is reduced to 520 DEG C, then in clean Grown on Sapphire Substrates low temperature GaN
Nucleating layer, nucleating layer thickness is 20nm, and growth pressure is 400Torr；
Step 3：Reaction chamber temperature is increased to 950 DEG C, NH is passed through in temperature-rise period3Gas is to prevent GaN nucleating layers complete
It is complete to decompose, metal organic source TMGa is then passed to, the GaN layer of the 3D structures of growth regulation one is started in GaN nucleation layer surfaces, growth is thick
Spend for 200nm, growth pressure is 400Torr, and the GaN layer of the first 3D structures includes little GaN islands and great GaN islands；
Step 4：Reaction chamber temperature is increased to 1030 DEG C, NH is passed through in temperature-rise period3Gas is to prevent the first 3D structures
GaN layer decompose, heating terminate after close NH3Gas is passed through, and is only passed through H2Gas is carried out to the GaN layer of the first 3D structures
10min is handled, in the process H2Gas can be performed etching to the GaN layer of 3D structures, small in the GaN layer of the first 3D structures
GaN islands can be etched away, and great GaN islands are then remained；
Step 5：Reaction chamber temperature is reduced to 950 DEG C, NH is passed through3Gas and metal organic source TMGa, in H2At gas
The GaN layer 500nm of the 3D structures of continued growth the 2nd in the GaN layer of 3D structures after reason, growth pressure is 400Torr, is expanded
Big 3D structure GaNs layer；
Step 6：Reaction chamber temperature is increased to 1050 DEG C, mushroomed out in the GaN layer of the 3D structures of expansion undoped with
GaN so that 3D island structures heal rapidly, and ultimately form interior void than more uniform the flat engraved structure in surface
GaN rough layers, growth thickness is 1um, and growth pressure is 50Torr；
Step 7：The GaN layer of unintentional doping is grown, thickness is 1um, and growth temperature is 1050 DEG C, and growth pressure is
50Torr；
Step 8：The GaN layer of Si doping is grown, this layer of carrier concentration is 1018cm-3, thickness is 1um, growth temperature
For 1050 DEG C, growth pressure is 50Torr；
Step 9：The multiple quantum well active layer in 3 cycles is grown, wherein barrier layer is GaN, and well layer is InGaN, In groups
Divide and be calculated as 30% with mass fraction, well layer thickness is 2nm, growth temperature is 700 DEG C, and barrier layer thickness is 8nm, growth temperature
For 800 DEG C, pressure is 200Torr in growth course；
Step 10：Grow Al components in the thick p-AlGaN electronic barrier layers of 20nm, the layer and be calculated as 10% with mass fraction,
Hole concentration is 1017cm-3, growth temperature is 850 DEG C, and pressure is 50Torr；
Step 11：The GaN layer of Mg doping is grown, thickness is 100nm, and growth temperature is 850 DEG C, and growth pressure is
100Torr, hole concentration is 1017cm-3；
Step 12：After epitaxial growth terminates, the temperature of reaction chamber is down to 650 DEG C, moved back in nitrogen atmosphere
Fire processing 15min, is then down to room temperature, terminates growth, obtain epitaxial wafer, epitaxial wafer is after over cleaning, deposition, photoetching and etching
Single small-size chips are made.
Embodiment two：
A kind of preparation method of high-luminous-efficiency GaN-based LED epitaxial wafer, comprises the following steps：
Step one：Sapphire Substrate is carried out to temperature in cleaning substrate surface, reaction chamber in MOCVD reaction chamber atmosphere of hydrogen
Spend for 1100 DEG C, the time is 5min；
Step 2：Reaction chamber temperature is reduced to 550 DEG C, then in clean Grown on Sapphire Substrates low temperature GaN
Nucleating layer, nucleating layer thickness is 40nm, and growth pressure is 700Torr；
Step 3：Reaction chamber temperature is increased to 1000 DEG C, NH is passed through in temperature-rise period3Gas is to prevent GaN nucleating layers
Decompose completely, then pass to metal organic source TMGa, the GaN layer of the 3D structures of growth regulation one is started in GaN nucleation layer surfaces, grow
Thickness is 300nm, and growth pressure is 700Torr, and the GaN layer of the first 3D structures includes little GaN islands and great GaN islands；
Step 4：Reaction chamber temperature is increased to 1050 DEG C, NH is passed through in temperature-rise period3Gas is to prevent the first 3D structures
GaN layer decompose, heating terminate after close NH3Gas is passed through, and is only passed through H2Gas is carried out to the GaN layer of the first 3D structures
9min is handled, in the process H2Gas can be performed etching to the GaN layer of 3D structures, small GaN in the GaN layer of the first 3D structures
Island can be etched away, and great GaN islands are then remained；
Step 5：Reaction chamber temperature is reduced to 1000 DEG C, NH is passed through3Gas and metal organic source TMGa, in H2At gas
The GaN layer 1000nm of the 3D structures of continued growth the 2nd in the GaN layer of 3D structures after reason, growth pressure is 700Torr, is expanded
Big 3D structure GaNs layer；
Step 6：Reaction chamber temperature is increased to 1200 DEG C, mushroomed out in the GaN layer of the 3D structures of expansion undoped with
GaN so that 3D island structures heal rapidly, and ultimately form interior void than more uniform the flat engraved structure in surface
GaN rough layers, growth thickness is 2um, and growth pressure is 300Torr；
Step 7：The GaN layer of unintentional doping is grown, thickness is 2um, and growth temperature is 1200 DEG C, and growth pressure is
300Torr；
Step 8：The GaN layer of Si doping is grown, this layer of carrier concentration is 1019cm-3, thickness is 3um, growth temperature
For 1200 DEG C, growth pressure is 300Torr；
Step 9：The multiple quantum well active layer in 4 cycles is grown, wherein barrier layer is GaN, and well layer is InGaN, In groups
Divide and be calculated as 10% with mass fraction, well layer thickness is 5nm, growth temperature is 800 DEG C, and barrier layer thickness is 13nm, growth temperature
Spend for 950 DEG C, pressure is 500Torr in growth course；
Step 10：Grow Al components in the thick p-AlGaN electronic barrier layers of 50nm, the layer and be calculated as 20% with mass fraction,
Hole concentration is 1018cm-3, growth temperature is 1000 DEG C, and pressure is 300Torr；
Step 11：The GaN layer of Mg doping is grown, thickness is 300nm, and growth temperature is 1000 DEG C, and growth pressure is
500Torr, hole concentration is 1018cm-3；
Step 12：After epitaxial growth terminates, the temperature of reaction chamber is down to 800 DEG C, annealed in nitrogen atmosphere
5min is handled, room temperature is then down to, terminates growth, obtains epitaxial wafer, epitaxial wafer is made after over cleaning, deposition, photoetching and etching
Into single small-size chips.
Embodiment three：
A kind of preparation method of high-luminous-efficiency GaN-based LED epitaxial wafer, comprises the following steps：
Step one：Sapphire Substrate is carried out to temperature in cleaning substrate surface, reaction chamber in MOCVD reaction chamber atmosphere of hydrogen
Spend for 1080 DEG C, the time is 7min；
Step 2：Reaction chamber temperature is reduced to 530 DEG C, then in clean Grown on Sapphire Substrates low temperature GaN
Nucleating layer, nucleating layer thickness is 30nm, and growth pressure is 500Torr；
Step 3：Reaction chamber temperature is increased to 960 DEG C, NH is passed through in temperature-rise period3Gas is to prevent GaN nucleating layers complete
It is complete to decompose, metal organic source TMGa is then passed to, the GaN layer of the 3D structures of growth regulation one is started in GaN nucleation layer surfaces, growth is thick
Spend for 220nm, growth pressure is 500Torr, and the GaN layer of the first 3D structures includes little GaN islands and great GaN islands；
Step 4：Reaction chamber temperature is increased to 1070 DEG C, NH is passed through in temperature-rise period3Gas is to prevent the first 3D structures
GaN layer decompose, heating terminate after close NH3Gas is passed through, and is only passed through H2Gas is carried out to the GaN layer of the first 3D structures
9min is handled, in the process H2Gas can be performed etching to the GaN layer of 3D structures, small GaN in the GaN layer of the first 3D structures
Island can be etched away, and great GaN islands are then remained；
Step 5：Reaction chamber temperature is reduced to 960 DEG C, NH is passed through3Gas and metal organic source TMGa, in H2At gas
The GaN layer 700nm of continued growth 3D structures in the GaN layer of 3D structures after reason, growth pressure is 500Torr, is expanded
3D structure GaNs layer；
Step 6：Reaction chamber temperature is increased to 1100 DEG C, mushroomed out in the GaN layer of the 3D structures of expansion undoped with
GaN so that 3D island structures heal rapidly, and ultimately form interior void than more uniform the flat engraved structure in surface
GaN rough layers, growth thickness is 1.2um, and growth pressure is 120Torr；
Step 7：The GaN layer of unintentional doping is grown, thickness is 1.2um, and growth temperature is 1100 DEG C, and growth pressure is
120Torr；
Step 8：The GaN layer of Si doping is grown, this layer of carrier concentration is 3 × 1018cm-3, thickness is 2um, growth temperature
Spend for 1100 DEG C, growth pressure is 120Torr；
Step 9：The multiple quantum well active layer in 5 cycles is grown, wherein barrier layer is GaN, and well layer is InGaN, In groups
Divide and be calculated as 25% with mass fraction, well layer thickness is 3nm, growth temperature is 730 DEG C, and barrier layer thickness is 10nm, growth temperature
For 850 DEG C, pressure is 300Torr in growth course；
Step 10：Grow Al components in the thick p-AlGaN electronic barrier layers of 30nm, the layer and be calculated as 12% with mass fraction,
Hole concentration is 2 × 1017cm-3, growth temperature is 930 DEG C, and pressure is 120Torr；
Step 11：The GaN layer of Mg doping is grown, thickness is 200nm, and growth temperature is 930 DEG C, and growth pressure is
400Torr, hole concentration is 3 × 1017cm-3；
Step 12：After epitaxial growth terminates, the temperature of reaction chamber is down to 700 DEG C, moved back in nitrogen atmosphere
Fire processing 12min, is then down to room temperature, terminates growth, obtain epitaxial wafer, epitaxial wafer is after over cleaning, deposition, photoetching and etching
Single small-size chips are made.
Example IV:
A kind of preparation method of high-luminous-efficiency GaN-based LED epitaxial wafer, comprises the following steps：
Step one：Sapphire Substrate is carried out to temperature in cleaning substrate surface, reaction chamber in MOCVD reaction chamber atmosphere of hydrogen
Spend for 1070 DEG C, the time is 8min；
Step 2：Reaction chamber temperature is reduced to 540 DEG C, then in clean Grown on Sapphire Substrates low temperature GaN
Nucleating layer, nucleating layer thickness is 25nm, and growth pressure is 600Torr；
Step 3：Reaction chamber temperature is increased to 970 DEG C, NH is passed through in temperature-rise period3Gas is to prevent GaN nucleating layers complete
It is complete to decompose, metal organic source TMGa is then passed to, the GaN layer of the 3D structures of growth regulation one is started in GaN nucleation layer surfaces, growth is thick
Spend for 240nm, growth pressure is 600Torr, and the GaN layer of the first 3D structures includes little GaN islands and great GaN islands；
Step 4：Reaction chamber temperature is increased to 1090 DEG C, NH is passed through in temperature-rise period3Gas is to prevent the first 3D structures
GaN layer decompose, heating terminate after close NH3Gas is passed through, and is only passed through H2Gas is carried out to the GaN layer of the first 3D structures
7min is handled, in the process H2Gas can be performed etching to the GaN layer of 3D structures, small GaN in the GaN layer of the first 3D structures
Island can be etched away, and great GaN islands are then remained；
Step 5：Reaction chamber temperature is reduced to 970 DEG C, NH is passed through3Gas and metal organic source TMGa, in H2At gas
The GaN layer 800nm of the 3D structures of continued growth the 2nd in the GaN layer of 3D structures after reason, growth pressure is 600Torr, is expanded
Big 3D structure GaNs layer；
Step 6：Reaction chamber temperature is increased to 1150 DEG C, mushroomed out in the GaN layer of the 3D structures of expansion undoped with
GaN so that 3D island structures heal rapidly, and ultimately form interior void than more uniform the flat engraved structure in surface
GaN rough layers, growth thickness is 1.4um, and growth pressure is 190Torr；
Step 7：The GaN layer of unintentional doping is grown, thickness is 1.4um, and growth temperature is 1150 DEG C, and growth pressure is
190Torr；
Step 8：The GaN layer of Si doping is grown, this layer of carrier concentration is 5 × 1018cm-3, thickness is 1.5um, growth
Temperature is 1150 DEG C, and growth pressure is 190Torr；
Step 9：The multiple quantum well active layer in 6 cycles is grown, wherein barrier layer is GaN, and well layer is InGaN, In groups
Divide and be calculated as 15% with mass fraction, well layer thickness is 4nm, growth temperature is 780 DEG C, and barrier layer thickness is 9nm, growth temperature
For 920 DEG C, pressure is 450Torr in growth course；
Step 10：Grow Al components in the thick p-AlGaN electronic barrier layers of 40nm, the layer and be calculated as 14% with mass fraction,
Hole concentration is 5 × 1017cm-3, growth temperature is 970 DEG C, and pressure is 190Torr；
Step 11：The GaN layer of Mg doping is grown, thickness is 260nm, and growth temperature is 970 DEG C, and growth pressure is
300Torr, hole concentration is 8 × 1017cm-3；
Step 12：After epitaxial growth terminates, the temperature of reaction chamber is down to 780 DEG C, annealed in nitrogen atmosphere
7min is handled, room temperature is then down to, terminates growth, obtains epitaxial wafer, epitaxial wafer is made after over cleaning, deposition, photoetching and etching
Into single small-size chips.
Embodiment five:
A kind of preparation method of high-luminous-efficiency GaN-based LED epitaxial wafer, comprises the following steps：
Step one：Sapphire Substrate is carried out to temperature in cleaning substrate surface, reaction chamber in MOCVD reaction chamber atmosphere of hydrogen
Spend for 1090 DEG C, the time is 6min；
Step 2：Reaction chamber temperature is reduced to 545 DEG C, then in clean Grown on Sapphire Substrates low temperature GaN
Nucleating layer, nucleating layer thickness is 35nm, and growth pressure is 650Torr；
Step 3：Reaction chamber temperature is increased to 980 DEG C, NH is passed through in temperature-rise period3Gas is to prevent GaN nucleating layers complete
It is complete to decompose, metal organic source TMGa is then passed to, the GaN layer of the 3D structures of growth regulation one is started in GaN nucleation layer surfaces, growth is thick
Spend for 260nm, growth pressure is 550Torr, and the GaN layer of the first 3D structures includes little GaN islands and great GaN islands；
Step 4：Reaction chamber temperature is increased to 1110 DEG C, NH is passed through in temperature-rise period3Gas is to prevent the first 3D structures
GaN layer decompose, heating terminate after close NH3Gas is passed through, and is only passed through H2Gas is carried out to the GaN layer of the first 3D structures
5min is handled, in the process H2Gas can be performed etching to the GaN layer of 3D structures, small GaN in the GaN layer of the first 3D structures
Island can be etched away, and great GaN islands are then remained；
Step 5：Reaction chamber temperature is reduced to 980 DEG C, NH is passed through3Gas and metal organic source TMGa, in H2At gas
The GaN layer 1000nm of the 3D structures of continued growth the 2nd in the GaN layer of 3D structures after reason, growth pressure is 650Torr, is expanded
Big 3D structure GaNs layer；
Step 6：Reaction chamber temperature is increased to 1080 DEG C, mushroomed out in the GaN layer of the 3D structures of expansion undoped with
GaN so that 3D island structures heal rapidly, and ultimately form interior void than more uniform the flat engraved structure in surface
GaN rough layers, growth thickness is 1.6um, and growth pressure is 260Torr；
Step 7：The GaN layer of unintentional doping is grown, thickness is 1.6um, and growth temperature is 1080 DEG C, and growth pressure is
260Torr；
Step 8：The GaN layer of Si doping is grown, this layer of carrier concentration is 7 × 1018cm-3, thickness is 2.5um, growth
Temperature is 1080 DEG C, and growth pressure is 260Torr；
Step 9：The multiple quantum well active layer in 5 cycles is grown, wherein barrier layer is GaN, and well layer is InGaN, In groups
Divide and be calculated as 20% with mass fraction, well layer thickness is 3nm, growth temperature is 760 DEG C, and barrier layer thickness is 12nm, growth temperature
Spend for 890 DEG C, pressure is 400Torr in growth course；
Step 10：Grow Al components in the thick p-AlGaN electronic barrier layers of 30nm, the layer and be calculated as 16% with mass fraction,
Hole concentration is 3 × 1017cm-3, growth temperature is 950 DEG C, and pressure is 260Torr；
Step 11：The GaN layer of Mg doping is grown, thickness is 220nm, and growth temperature is 950 DEG C, and growth pressure is
200Torr, hole concentration is 5 × 1017cm-3；
Step 12：After epitaxial growth terminates, the temperature of reaction chamber is down to 750 DEG C, moved back in nitrogen atmosphere
Fire processing 10min, is then down to room temperature, terminates growth, obtain epitaxial wafer, epitaxial wafer is after over cleaning, deposition, photoetching and etching
Single small-size chips are made.
The engraved structure GaN rough layer process schematics that Fig. 3-Fig. 6 grows for the present invention, wherein Fig. 3 is in extension
Schematic diagram on piece after the GaN layers of the 3D structures of growth regulation one, the size on GaN islands and distribution are all uneven as shown in Figure 3；Fig. 4
For H2Schematic diagram after the GaN layers of the 3D structures of high-temperature process the first, little GaN islands are by H as shown in Figure 42Etch away, the number on island
Quantitative change is few, and size is evenly；Fig. 5 is the schematic diagram after the GaN layers of the 2nd 3D structures of growth, preferred growth when GaN grows
In the position with GaN islands, other positions are slow-growing, eventually form larger-size, size and are distributed more uniform GaN
Three-dimensional island structure.The empty schematic diagram that Fig. 6 is internally formed after quickly merging for the GaN layers of 3D structures.The interior void compares
Uniformly the flat engraved structure GaN rough layers in surface, can reduce total internal reflection, be conducive to improving GaN base LED light extraction
Efficiency.In addition using the GaN 3D structure growth techniques of two steps, help to change the direction of growth of dislocation so that the position of active area
Dislocation density is reduced, and improves the crystal mass of epitaxial wafer.
Fig. 7 is is respectively adopted made by the epitaxial wafer that epitaxial wafer and the commonsense method of the method growth that the present invention is provided grow
LED chip optical output power profiles versus figure.Test condition is randomly selects 180 samples, and chip size 8x10mil is surveyed
Try electric current 20mA.The chip optical output power average of conventional method is used for 18.1mW, and uses the core of the method provided by the present invention
Piece optical output power average is 22.9mW, i.e., the chip optical output power of the method growth provided using the present invention compares commonsense method
The LED chip optical output power of formation improves about 26.5%.
Claims (1)
1. a kind of preparation method of GaN-based LED epitaxial wafer, it is characterised in that comprise the following steps：
Step one：Sapphire Substrate is subjected to substrate surface cleaning in reaction chamber atmosphere of hydrogen, reaction cavity temperature is 1060-
1100 DEG C, the time is 5min-10min；
Step 2：Reaction chamber temperature is reduced to 520-550 DEG C, then in clean Grown on Sapphire Substrates low temperature GaN
Nucleating layer, nucleating layer thickness is 20-40nm, and growth pressure is 400-700Torr；
Step 3：Reaction chamber temperature is increased to 950-1000 DEG C, and stable 2min, the high annealing of GaN nucleating layers is carried out, this
During be passed through NH3Gas then passes to metal organic source TMGa to prevent GaN nucleating layers from decomposing completely, in GaN nucleating layer tables
Face starts the GaN layer of the 3D structures of growth regulation one, and growth thickness is 200-300nm, and growth pressure is 400-700Torr, the first 3D
The GaN layer of structure includes little GaN islands and great GaN islands；
Step 4：Reaction chamber temperature is increased in 1030-1110 DEG C, temperature-rise period and is passed through NH3Gas is to prevent the first 3D structures
GaN layer decompose, heating terminate after close NH3Gas is passed through, and is only passed through H2Gas is carried out to the GaN layer of the first 3D structures
5-10min is handled, in the process H2Gas can be performed etching to the GaN layer of 3D structures, small in the GaN layer of the first 3D structures
GaN islands can be etched away, and great GaN islands are then remained；
Step 5：Reaction chamber temperature is reduced to 950-1000 DEG C, NH is passed through3Gas and metal organic source TMGa, in H2At gas
The GaN layer 500-1000nm of the 3D structures of continued growth the 2nd in the GaN layer of 3D structures after reason, growth pressure is 400-
700Torr, the 3D structure GaNs layer expanded；
Step 6：Reaction chamber temperature is increased to 1050-1200 DEG C, mushrooms out and does not mix in the GaN layer of the 3D structures of expansion
Miscellaneous GaN so that 3D island structures heal rapidly, and ultimately form interior void than more uniform the flat engraved structure in surface
GaN rough layers, growth thickness be 1 ~ 2um, growth pressure is 50-300Torr；
Step 7：The GaN layer of unintentional doping is grown, thickness is 1 ~ 2um, and growth temperature is 1050-1200 DEG C, and growth pressure is
50-300Torr；
Step 8：The GaN layer of Si doping is grown, this layer of carrier concentration is 1018-1019cm-3, thickness is 1-3um, growth temperature
Spend for 1050-1200 DEG C, growth pressure is 50-300Torr；
Step 9：The multiple quantum well active layer in 3-6 cycle is grown, wherein barrier layer is GaN, and well layer is InGaN, In components
10-30% is calculated as with mass fraction, well layer thickness is 2-5nm, and growth temperature is 700-800 DEG C, and barrier layer thickness is 8-
13nm, growth temperature is 800-950 DEG C, and pressure is 200-500Torr in growth course；
Step 10：Grow Al components in the thick p-type AlGaN electronic barrier layers of 20-50nm, the layer and 10- is calculated as with mass fraction
20%, hole concentration is 1017-1018cm-3, growth temperature is 850 DEG C -1000 DEG C, and pressure is 50-300Torr；
Step 11：The GaN layer of Mg doping is grown, thickness is 100-300nm, and growth temperature is 850-1000 DEG C, growth pressure
For 100-500Torr, hole concentration is 1017-1018cm-3；
Step 12：After epitaxial growth terminates, the temperature of reaction chamber is down to 650-800 DEG C, moved back in nitrogen atmosphere
Fire processing 5-15min, is then down to room temperature, terminates growth, obtain epitaxial wafer；Above-mentioned little GaN islands and great GaN islands does not have
Clear and definite size definition, simply size little GaN islands are easily etched away in etching process, therefore the GaN islands being etched away
For little GaN islands, the GaN islands Wei great GaN islands remained.
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