CN105720139B - Improve the epitaxial growth method of iii-nitride light emitting devices p-type doping concentration - Google Patents
Improve the epitaxial growth method of iii-nitride light emitting devices p-type doping concentration Download PDFInfo
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- 230000012010 growth Effects 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 21
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 claims abstract description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 5
- 230000004888 barrier function Effects 0.000 claims abstract description 4
- 239000000758 substrate Substances 0.000 claims abstract description 4
- 239000011777 magnesium Substances 0.000 claims description 34
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 12
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 12
- 230000004907 flux Effects 0.000 claims description 10
- 229910052749 magnesium Inorganic materials 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 13
- 150000004767 nitrides Chemical class 0.000 abstract description 10
- 239000000370 acceptor Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 3
- ZXVONLUNISGICL-UHFFFAOYSA-N 4,6-dinitro-o-cresol Chemical class CC1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1O ZXVONLUNISGICL-UHFFFAOYSA-N 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000004886 process control 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
- H01L33/0075—Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01L21/0254—Nitrides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01L21/0257—Doping during depositing
- H01L21/02584—Delta-doping
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- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
The epitaxial growth method of iii-nitride light emitting devices p-type doping concentration is improved, is related to nitride epitaxial technical field, the present invention grown buffer layer, N-type layer, light-emitting active layer, electronic barrier layer, P-type layer and contact layer successively on substrate, it is characterised in that：In N2Under the atmosphere of ammonia, by controlling trimethyl indium flow multi ANN to form P-type layer, the P Al of formationXGa1‑XN material layers hole concentration can be significantly improved, and square resistance can obviously reduce, and the LED light electrical property based on this material layer can be obviously improved.
Description
Technical field
The present invention relates to nitride epitaxial technical field, is especially to provide one kind and is remarkably improved iii-nitride light emitting devices
（LED）The epitaxial growth method of p-type doping concentration.
Background technology
III group nitride material is obtained in recent years due to its wide application prospect in the field such as photoelectron and microelectronics
Extensive concern.Particularly in optoelectronic areas, have been widely used for making light emitting diode（LED）.LED with its small volume,
The advantages of long lifespan, energy-conserving and environment-protective etc. are peculiar, important role is play in visible ray and black light field.But with
AlXGa1-XThe p-type doping techniques of nitride luminescent material based on N (1 >=X >=0), but it is difficult to be broken through always, high hole
The p-type nitride luminescent material of concentration is difficult to obtain always, governs the development of nitride light-emitting device, in particular with Al groups
The raising divided, p-type doping become particularly difficult.But report display according to the study, following LED markets mainly will be divided into two
Part, a portion are so that towards the visible ray nitride LED based on general illumination, another part is innovated with high-tech
For the high Al contents deep ultraviolet LED of characteristic.Therefore, development of the raising of nitride p-type doping techniques to nitride LED plays
Vital effect.
Current nitride LED, typically with AlXGa1-XN is main p-type epitaxial material, in AlXGa1-XIn N Material growths
By being passed through two luxuriant magnesium（Cp2Mg）Carry out p-type doping.It is self-complementary caused by defect yet with low acceptor doping thing solubility
Repay effect and AlXGa1-XHigh Mg acceptor activation energy in N materials so that the P-Al of high hole concentrationXGa1-XN materials are difficult always
To obtain.By the way that to epitaxial growth temperature, pressure, the optimization of speed, hole concentration can be improved to a certain extent, in addition, passing through
Growth material superlattice structure carries out also can to a certain extent improving hole concentration, but existing doping skill with the technology of modulation
Art, still it is difficult to reach higher hole concentration.
P-Al at presentXGa1-XN growth typically uses uniform Mg doping techniques, i.e.,:It is passed through simultaneously into reative cell
TMGa/TMAl/NH3/Cp2Mg carries out whole P-AlXGa1-XThe growth of N layers, this growth technique are difficult to the P- for obtaining high hole concentration
AlXGa1-XN layers, govern the lifting of device photoelectric performance.
The content of the invention
The present invention is intended to provide a kind of improve AlXGa1-XThe epitaxial growth method of N p-type doping concentrations, to significantly improve P-
AlXGa1-XN material layer hole concentrations, lift LED light electrical property.
Grown buffer layer, N-type layer, light-emitting active layer, electronic barrier layer, P-type layer and the contact of the invention successively on substrate
Layer, it is characterised in that：In N2Under the atmosphere of ammonia, growth forms P-type layer, and step is as follows：
1）Under conditions of growth temperature is 900~1100 DEG C, the trimethyl gallium of uniform flux is passed through into reative cell
（TMGa）, uniform flux trimethyl aluminium（TMAl）With the trimethyl indium of variable-flow（TMIn）, grow one layer of AlXGa1-XN thin layers；
The trimethyl indium（TMIn）Flow priority in this stage be respectively identical uniform flux, intermediate flow at this stage
Amount linearly becomes big by becoming zero greatly, then by zero；
2）Turn off the trimethyl gallium being passed through into reative cell（TMGa）, trimethyl aluminium（TMAl）And trimethyl indium（TMIn）,
Carry out 10~60s high temperature interrupt growth；In the high temperature interrupt growth course, growth temperature is linearly warming up to 950~
1150 DEG C, after warm 10~60s, then growth temperature is linearly cooled to 900~1100 DEG C；
3）Two luxuriant magnesium are passed through into reative cell（Cp2Mg）, growth temperature be 900~1100 DEG C under conditions of growth 1~
60s；
4）Repeat step 1）To 3）10~20 cycles；
5）Under conditions of growth temperature is 900~1100 DEG C, the luxuriant magnesium of two be passed through into reative cell is turned off, to reative cell
In be passed through the trimethyl gallium of uniform flux（TMGa）, uniform flux trimethyl aluminium（TMAl）With the trimethyl indium of variable-flow
（TMIn）, grow one layer of AlXGa1-XN thin layers；The trimethyl indium（TMIn）Flow in this stage linearly by becoming zero greatly；
6）Turn off the trimethyl gallium being passed through into reative cell（TMGa）, trimethyl aluminium（TMAl）And trimethyl indium（TMIn）,
Interruption of growth carries out 10~60s high-temperature baking；The high-temperature baking temperature is linearly warming up to 950~1150 DEG C, warm
After 10~60s, then growth temperature is linearly cooled to 900~1100 DEG C.
Pass through this special epitaxial growth method, P-AlXGa1-XN material layers hole concentration can significantly improve, square resistance
It can obviously reduce, the LED light electrical property based on this material layer can be obviously improved.
In step 1）In, control trimethyl indium（TMIn）The purpose of flow：
<1>By this flow design, In can give full play to the effect of surfactant, improve AlGaN crystal mass, subtract
The defects of few follow-up Mg is adulterated self-compensation mechanism, while improve the In deposition gone adsorption capacity, reduce In.
<2>TMIn flows are larger in the interface of close Mg doped layers, InN can be being formed close to interface, by step
2. after the process of high-temperature baking, In-N keys are easily broken off because its combination can be relatively low, and this will form more III races room to follow-up
The Mg of step 3. is captured, and greatly improves Mg doping efficiency.
In step 2）The middle process toasted using interruption of growth and raising high-temperature, can reach following purpose：
<1>High-temperature baking can parse and be incorporated to AlXGa1-XIn in N thin layers, In is reduced in AlXGa1-XIt is residual in N epitaxial layers
Stay, and In-N keys because its combine can relatively low, easy fracture under high temperature, high-temperature baking will form more III races room to subsequent step
3. Mg capture, greatly improve Mg doping efficiency.
<2>High-temperature baking, Mg can be improved toward AlXGa1-XThe diffusion of N layers.
In step 1）In be not passed through Mg and in step 3）In be individually passed through two luxuriant magnesium（Cp2Mg）, this detal doping techniques
The efficiency that Mg is incorporated to epitaxial layer can be improved, reduces the self-compensation mechanism of Mg acceptors.
Feature of the present invention：
1st, in AlXGa1-XIn the growth course of N layers, TMIn sources are passed through in the form of variable-flow, reaches and is passed through TMIn on a small quantity
The purpose in source, In can give full play to the effect of surfactant, improve AlGaN crystal mass, reduce lacking for follow-up Mg doping
Self-compensation mechanism is fallen into, while improves the In deposition gone adsorption capacity, reduce In.
2nd, using AlXGa1-XN thin layers/Mg/AlXGa1-XN laminate structures, the efficiency that Mg is incorporated to epitaxial layer can be improved, reduce Mg
The self-compensation mechanism of acceptor.
3、AlXGa1-XAfter the completion of N growths, organic source is closed, interruption of growth and the process of high-temperature baking is carried out, can parse
It is incorporated to AlXGa1-XIn in N thin layers, In is reduced in AlXGa1-XResidual in N epitaxial layers, while Mg can be improved toward AlXGa1-XN layers
Diffusion.
4th, TMIn flows are larger in the interface close to Mg doped layers, can form InN in interface, by step 2. high temperature
After the process of baking, In-N keys because it is combined can be relatively low, be easily broken off, 3. this will form more III races room to subsequent step
Mg capture, greatly improve Mg doping efficiency.
In a word, the detal doping techniques that the present invention is aided in by In, while introduce the mistake that interruption of growth carries out high-temperature baking
Journey, and special design is carried out to In flows, Mg incorporation efficiency is significantly improved, while reduce In in P-AlXGa1-XN
Being incorporated in layer, improves the photoelectric properties of device.
Further, step 1 of the present invention）The Al of middle growthXGa1-XThe thickness of N thin layers is 5~25nm.
The step 5）The Al of middle growthXGa1-XThe thickness of N thin layers is 5~25nm.
Brief description of the drawings
Fig. 1 is the product structure schematic diagram that the present invention is formed.
Fig. 2 is process-control chart of the present invention in growing P-type layer.
Embodiment
A kind of iii-nitride light emitting devices epitaxial growth method for improving p-type doping concentration, as shown in Figure 1：In substrate 1
On grown buffer layer 2, N-type layer 3, light-emitting active layer 4, electronic barrier layer 5, P-type layer 6 and contact layer 7 successively.
Wherein P-type layer 6 is AlXGa1-XN layers, whole production process is except in N2And ammonia（NH3）Atmosphere under carry out, and such as
Shown in Fig. 2, the specific growing method of the layer is as follows：
1st, ammonia is passed through into reative cell（NH3）, trimethyl gallium（TMGa）, trimethyl aluminium（TMAl）, grow one layer
AlXGa1-XN thin layers, 5~25nm of growth thickness, 900 DEG C~1100 DEG C of growth temperature.
In the growth course of this layer, a small amount of trimethyl indium is also passed through（TMIn）：Trimethyl indium（TMIn）Flow exist
In the stage is respectively identical uniform flux one after another, and middle flow at this stage linearly becomes by becoming zero greatly, then by zero
Greatly.
2nd, trimethyl gallium is closed（TMGa）, trimethyl aluminium（TMAl）And trimethyl indium（TMIn）Valve, carry out high temperature interrupt
Grow 10~60s.
In the high temperature interrupt growth course, growth temperature is linearly warming up to 950~1150 DEG C, warm 10~60s
Afterwards, then by growth temperature 900~1100 DEG C are linearly cooled to.
3rd, two luxuriant magnesium are opened（Cp2Mg）Valve, grow 1~60s under conditions of being 900~1100 DEG C in growth temperature.
4th, above step 1 is repeated）To 3）10~20 cycles.
5th, two luxuriant magnesium valves are closed, open trimethyl gallium（TMGa）And trimethyl aluminium（TMAl）Valve, one layer of regrowth
AlXGa1-XN thin layers, 5~25nm of growth thickness, 900~1100 DEG C of growth temperature.
In the growth course of this layer, a small amount of trimethyl indium is also passed through（TMIn）：Trimethyl indium（TMIn）Flow exist
Linearly by becoming zero greatly in the stage.
6th, trimethyl gallium is closed（TMGa）, trimethyl aluminium（TMAl）And trimethyl indium（TMIn）Valve, interruption of growth, carry out
10~60s of high-temperature baking.
High-temperature baking temperature is linearly warming up to 950~1150 DEG C, after warm 10~60s, then by growth temperature is in line
Property is cooled to 900~1100 DEG C.
Claims (3)
1. the epitaxial growth method of iii-nitride light emitting devices p-type doping concentration is improved, grown buffer layer, N successively on substrate
Type layer, light-emitting active layer, electronic barrier layer, P-type layer and contact layer, it is characterised in that：In N2Under the atmosphere of ammonia, shape is grown
It is as follows into P-type layer, step：
1）Under conditions of growth temperature is 900~1100 DEG C, trimethyl gallium, the uniform flow of uniform flux are passed through into reative cell
The trimethyl aluminium of amount and the trimethyl indium of variable-flow, grow one layer of AlXGa1-XN thin layers；The flow of the trimethyl indium is in the rank
Priority in section is respectively identical uniform flux, and middle flow at this stage linearly becomes big by becoming zero greatly, then by zero；
2）The trimethyl gallium being passed through into reative cell, trimethyl aluminium and trimethyl indium are turned off, carries out 10~60s high temperature interrupt life
It is long；In the high temperature interrupt growth course, growth temperature is linearly warming up to 950~1150 DEG C, after warm 10~60s, then
Growth temperature is linearly cooled to 900~1100 DEG C；
3）Two luxuriant magnesium are passed through into reative cell, grow 1~60s under conditions of being 900~1100 DEG C in growth temperature；
4）Repeat step 1）To 3）10~20 cycles；
5）Under conditions of growth temperature is 900~1100 DEG C, the luxuriant magnesium of two be passed through into reative cell is turned off, is led into reative cell
Enter the trimethyl indium of the trimethyl gallium of uniform flux, the trimethyl aluminium of uniform flux and variable-flow, grow one layer of AlXGa1-XN is thin
Layer；The flow of the trimethyl indium is in this stage linearly by becoming greatly zero；
6）The trimethyl gallium being passed through into reative cell, trimethyl aluminium and trimethyl indium are turned off, interruption of growth, carries out 10~60s's
High-temperature baking；The high-temperature baking temperature is linearly warming up to 950~1150 DEG C, after warm 10~60s, then by growth temperature
Linearly it is cooled to 900~1100 DEG C.
2. epitaxial growth method according to claim 1, it is characterised in that the step 1）The Al of middle growthXGa1-XN thin layers
Thickness be 5~25nm.
3. epitaxial growth method according to claim 1, it is characterised in that the step 5）The Al of middle growthXGa1-XN thin layers
Thickness be 5~25nm.
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| CN107887255B (en) * | 2017-09-18 | 2020-10-02 | 中国电子科技集团公司第五十五研究所 | High-resistance GaN film epitaxial growth method |
| CN111261494A (en) * | 2018-11-30 | 2020-06-09 | 东泰高科装备科技有限公司 | P-type GaAs layer and epitaxial growth method thereof, GaAs solar cell and preparation method |
| CN109888064B (en) * | 2019-01-24 | 2020-07-07 | 华灿光电（浙江）有限公司 | Growth method of light emitting diode epitaxial wafer |
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