CN1758456A - Method for growing InGaN/GaN quantum hydrolazium LED device structure on beta digallium trioxide substrate - Google Patents
Method for growing InGaN/GaN quantum hydrolazium LED device structure on beta digallium trioxide substrate Download PDFInfo
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- CN1758456A CN1758456A CNA2005100948804A CN200510094880A CN1758456A CN 1758456 A CN1758456 A CN 1758456A CN A2005100948804 A CNA2005100948804 A CN A2005100948804A CN 200510094880 A CN200510094880 A CN 200510094880A CN 1758456 A CN1758456 A CN 1758456A
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- 239000000758 substrate Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 19
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 title 1
- 239000000463 material Substances 0.000 claims abstract description 42
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000012159 carrier gas Substances 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 16
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract 6
- 238000000137 annealing Methods 0.000 claims description 12
- 229910052733 gallium Inorganic materials 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 4
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical group C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 4
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 229910052738 indium Inorganic materials 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001194 electroluminescence spectrum Methods 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000000103 photoluminescence spectrum Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000004907 flux Effects 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- -1 organo indium Chemical compound 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000000927 vapour-phase epitaxy Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 150000007516 brønsted-lowry acids Chemical class 0.000 description 1
- 150000007528 brønsted-lowry bases Chemical class 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 238000001657 homoepitaxy Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
This invention relates to a method for growing InGaN/GaN quanta traps on a beta-Ga<SUB>2</SUB>O<SUB>3</SUB> substrate material, which carries out heat treatment to the material of said substrate under 500-1050deg.C in the MOCVD system to inlet carrier gas N<SUB>2</SUB>, ammonia and a metallic organic source to synthesize and grow a low temperature buffer material on said substrate by controlling the carrier gas, the source gas flow and the grown temperature, then dopes Si to it to grow a GaN of type N under the temperature of 500-1050deg.C after growing the GaN buffer material with the MOCVD method then grows GaN/InGaN multiple quanta traps of 5-10 periods and grows a layer of P-type GaN to form the LED component structure to be annealed and activated under 600-800deg.C and 0.1-1 hour.
Description
Technical field
The present invention relates at a kind of novel substrate β-Ga
2O
3With the method for MOCVD (metal organic-matter chemical vapor phase epitaxy) technology growth GaN/InGaN quantum well LED, especially utilize the MOCVD technology on the material at β-Ga
2O
3Growing InGaN on the backing material/GaN quantum well LED device architecture technology.
Background technology
β-Ga
2O
3Be a kind of transparent conductor, the scope that its transparency range can be from the visible light to the ultraviolet light, and its intrinsic property has n type conductivity.Its energy gap is Eg=4.8eV (260nm).Because its this key property makes it have important application prospects in following short-wavelength light field of electronic devices.
Be the wide direct gap semiconductor of III V family of representative with GaN because have band gap wide (Eg=3.39eV), luminous efficiency height, electron drift saturated velocity height, thermal conductivity height, hardness is big, dielectric constant is little, chemical property is stable and radioresistance, characteristics such as high temperature resistant, in field of electronic devices such as opto-electronic devices such as high brightness blue light-emitting diode, blue laser and ultraviolet detector and radioresistance, high frequency, high temperature, high pressure huge application potential and vast market prospect are arranged, cause people's very big interest and extensive concern.GaN is the stock in the III group-III nitride, also is to study maximum III group nitride materials at present.The GaN material is very hard, and its chemical property is highly stable, at room temperature water insoluble, bronsted lowry acids and bases bronsted lowry, and its melting point is higher, is about 1700 ℃.The electrical properties of GaN is the principal element of decision device performance, and electronics room temperature mobility can reach 900cm2/ (Vs) at present.That the GaN sample of the involuntary doping of growing on Sapphire Substrate exists is higher, and (＞1018/cm3) n type background carrier concentration, the background n type carrier concentration of GaN sample can drop to about 1016/cm3 preferably now.Because n type background carrier concentration is higher, the technical barrier of preparation p type GaN sample had once once limited the development of GaN device.Nakamura etc. adopt the thermal anneal process technology, have better realized mixing the p-typeization of the GaN sample of Mg more easily, can prepare carrier concentration at the p-of 1011～1020/cm3 type GaN material at present.Entered since the nineties, because the employing of resilient coating technology and the breakthrough that the p type mixes technology, the research boom of GaN is grown up in the world, and obtained brilliant achievement.InGaN super brightness indigo plant, green light LED has been realized commercialization.
Backing material is very big for the crystal mass influence of heteroepitaxy GaN, to the Performance And Reliability generation significant effects of device.Shortage is one of main difficulty that influences GaN device maturation with the suitable backing material of GaN lattice match and heat compatibility.The most widely used at present C surface sapphire (c-plane-Al
2O
3) substrate is because its hardness is big, and natural insulation characterisitic makes in the LED postchannel process more complicated that becomes.Though it is tempting to carry out the homoepitaxy prospect on the GaN substrate, grow large scale GaN monocrystal and need time, seeking other desirable backing material also is one of effective way of dealing with problems.β-Ga
2O
3Be a kind of transparent conductor, the scope that its transparency range can be from the visible light to the ultraviolet light, and its intrinsic property has n type conductivity.Its energy gap is Eg=4.8eV (260nm).Because its this key property makes it may become a kind of backing material of very promising growing GaN.With β-Ga
2O
3Doing backing material utilizes MOCVD growing technology synthetically grown InGaN/GaN quantum-well materials and LED thereof not to appear in the newspapers as yet.
The applicant's patent application be to utilize the MOCVD growing technology at a kind of novel substrate β-Ga
2O
3The method of growing GaN on the material/InGaN quantum well LED especially utilizes the MOCVD technology at β-Ga
2O
3Growing InGaN on the backing material/GaN quantum well LED device architecture technology.The applicant utilizes the MOCVD growing technology at β-Ga first
2O
3Synthetically grown GaN thin-film material and InGaN/GaN quantum well LED device architecture on the backing material.This application is at β-Ga
2O
3Adopt MOCVD (metal organic-matter chemical vapor phase epitaxy) technology synthetically grown InGaN/GaN quantum well LED device architecture on the backing material, belong to first technically.
Summary of the invention
The present invention seeks to: at β-Ga
2O
3Adopt MOCVD (metal organic-matter chemical vapor phase epitaxy) technology synthetically grown InGaN/GaN quantum well LED device architecture on the substrate.
Technical solution of the present invention: at β-Ga
2O
3The method of growing InGaN on the backing material/GaN quantum well LED device architecture: at first, the β-Ga to growing in the MOCVD system
2O
3Substrate carries out material heat treatment under 500-1050 ℃ of temperature, feed carrier gas N in certain 500-1050 ℃ of temperature range again
2, ammonia and metal organic source, by the control carrier gas, parameters such as source gas flow and growth temperature are at β-Ga
2O
3Synthetically grown GaN material on the substrate, growth one deck doping content reaches 5*10 on this GaN material again
18Cm
-1N type GaN, then be respectively the GaN/InGaN quantum well in 5-10 the cycle of 15-20nm and 5-15nm respectively with 700-900 ℃ and 600-800 ℃ of growth bed thickness, one deck doping content of growing at last reaches 3*10
17Cm
-1The LED device architecture of P type GaN layer.And to this structure in the activation of annealing of 600-800 ℃ of temperature and 0.1-1 hour annealing time.
Mechanism of the present invention and technical characterstic:
Utilize the MOCVD growing technology at β-Ga
2O
3Synthetically grown GaN thin-film material and InGaN/GaN quantum well LED device architecture on the substrate.β-Ga to growing in the MOCVD system
2O
3Substrate carries out material heat treatment under 500-1050 ℃ of temperature, then or feed ammonia and carry out surfaces nitridedly, feed carrier gas N in certain 500-1050 ℃ of temperature range again
2, ammonia and metal organic source, by the control carrier gas, parameters such as source gas flow and growth temperature are at β-Ga
2O
3Synthetically grown GaN material on the substrate, again on this GaN material with 500-1050 ℃ of GaN/InGaN quantum well structure by mixing Si growth N type layer GaN and being respectively 5-10 the cycle of 15-20nm and 5-15nm respectively with 700-900 ℃ and 600-800 ℃ of growth bed thickness, pass through the LED device architecture of Mg doped growing one deck P type GaN at last.N type layer GaN concentration is 5*10
18Cm
-1, P type layer GaN concentration is 3*10
17Cm
-1And to this structure in the activation of annealing of 600-800 ℃ of temperature and 0.1-1 hour annealing time.Thereby form InGaN/GaN quantum well LED device architecture.
Wherein, β-Ga
2O
3The employing of substrate, β-Ga
2O
3Growing GaN resilient coating on the substrate, N type layer GaN, the GaN/InGaN quantum well structure in 5-10 cycle and P type layer GaN, and β-Ga
2O
3Thermal anneal process before the substrate growth, the thermal annealing temperature, the temperature control of growth material and the annealing activation technology of P type layer GaN are keys of the present invention.
The present invention is at β-Ga
2O
3The optimization growth conditions scope of growing GaN and InGaN/GaN quantum well LED device architecture is shown in Table 1 on the substrate.
Table 1. is at β-Ga
2O
3The optimization growth conditions scope of growing GaN on the substrate
| Growth | Growth temperature (℃ | Pressure (Torr) | The V/III ratio | Material | Growth atmosphere |
| Nucleation | 500-1050 | 0-500 | - | β-Ga 2O 3Substrate | Nitrogen |
| Buffering | 500-1050 | 0-500 | 500-300 | GaN | Nitrogen |
| The N type | 500-1050 | 0-500 | 500-300 | N type GaN | Nitrogen |
| Growth | GaN500-105 | 0-500 | 500-300 | The GaN/InGaN volume | Nitrogen |
| InGaN600-8 | 0-500 | 500-300 | Nitrogen | ||
| The P type | 800-1100 | 0-500 | 500-300 | P type GaN | Nitrogen |
| P type layer activates in the annealing of 600-800 ℃ of temperature and 0.1-1 hour annealing time | |||||
Description of drawings
Fig. 1 is InGaN/GaN quantum well LED device architecture figure of the present invention.In this structure, with β-Ga
2O
3As backing material, on this substrate, grow GaN as being resilient coating, on this resilient coating, grow again N type layer GaN and InGaN/GaN Multiple Quantum Well, the LED device architecture of one deck P type GaN that grows at last.Wherein the InGaN/GaN multi-quantum pit structure is: the InGaN Multiple Quantum Well of the GaN in 5-10 cycle and 15-20nmm.Thereby form InGaN/GaN quantum well LED device architecture.
Fig. 2 is that the present invention is at β-Ga
2O
3The XRD scintigram of Grown GaN on the substrate.As can be seen from the figure,, a plurality of β-Ga appear in the XRD scintigram
2O
3The substrate peak.And (0002) GaN peak position of growth is spent 34.64 thereon.XRD analysis proof GaN film thickness and quality are good.
Fig. 3 is that the present invention is at β-Ga
2O
3What grow on the substrate is InGaN/GaN quantum well LED device architecture LED tube core luminous photo, electroluminescence spectrum and the photoluminescence spectrum of resilient coating with (0002) GaN.As we can see from the figure our development with (0002) GaN be the sub-trap LED of the InGaN/GaN device of resilient coating luminous be blue green light (upper left corner accompanying drawing of Fig. 3).Its structure LED tube core electroluminescence spectrum (EL) is at the 537nm wave band, and photoluminescence spectrum (PL) is at the 529nm wave band.PL adopts the He-Cd laser to do excitaton source.The voltage that EL is added on the sample is 20V, and electric current is 0.7mA.
Embodiment
The present invention utilizes the MOCVD growing technology at β-Ga
2O
3Synthetically grown GaN thin-film material and InGaN/GaN quantum well LED device architecture on the substrate.Specifically comprise following a few step:
1, β-Ga in the MOCVD system to growing
2O
3Substrate carries out material heat treatment under 500-1050 ℃ of temperature, probable back feeds ammonia and carries out surfaces nitrided.Another embodiment is, feeds ammonia then and carry out surfaces nitridedly after above-mentioned heat treatment, and the time is also not have marked difference in 10,30,60 minutes.
2, after heat treatment (or through surfaces nitrided after) feeds carrier gas N 500-1050 ℃ of temperature range again
2, ammonia and metal organic gallium source and indium source, wherein gallium source and indium source flux remain unchanged, by the control carrier gas, parameters such as gallium source gas flow, by the control carrier gas, parameters such as source gas flow and growth temperature are at β-Ga
2O
3Synthetically grown GaN cushioning layer material on the substrate.
3, on this GaN material, mix Si growth N type layer GaN (1-1.5 μ m) again with 500-1050 ℃, then be respectively the GaN/InGaN quantum well structure in 5-10 the cycle of 15-20nm and 5-15nm respectively with 700-900 ℃ and the 600-800 ℃ bed thickness of growing, pass through the LED device architecture of Mg doped growing one deck P type GaN layer (200-500nm) at last.
4, organic gallium source is that trimethyl gallium stream is 1-50sccm.The organo indium source is that trimethyl indium stream is 50-200sccm.Carrier gas flux is 2-8slm.The ammonia flow that is added directly to substrate is 1-15slm.NH
3Flow is 3-8slm, and growth temperature is 500-1050 ℃.H
2Or N
2Or H
2And N
2Mist is as diluent gas, NH
3Gas is as nitrogenous source.H
2Or N
2Or H
2And N
2Air-fuel mixture enleanment throughput 2500-3500sccm, NH
3Gas 500-700sccm, the conversion zone temperature also can be 500-1050 ℃, growth time is can obtain A face GaN film completely under the condition of 8-20min.V/III refers to the mol ratio of N and Ga than being 500-3000.
5, wherein, β-Ga
2O
3The employing of substrate, and β-Ga
2O
3Thermal anneal process before the substrate growth, the control of thermal annealing temperature, the temperature control and the growth concentration of growth material are 5*10
18Cm
-1N type layer GaN, concentration is 3*10
17Cm
-1P type layer GaN, the GaN/InGaN quantum well LED device architecture and the nitrogen in 5-10 cycle of growth are keys of the present invention as carrier gas on growth back P type layer annealing activationary temperature and time and the lithium aluminate substrate.
Described organic gallium source is that trimethyl gallium stream is 1-50sccm, and the organo indium source is that trimethyl indium stream is 50-200sccm.According to this apparatus features, adopt the trimethyl gallium (indium) of different flow not have significantly difference, the speed of growth is different.Carrier gas flux is 2-8slm.The ammonia flow that is added directly to substrate is 1-15slm.NH
3Flow is 3-8slm, and growth temperature is 500-1050 ℃.
The further control of carrier band gas is H
2Or N
2Or H
2And N
2Mist is as diluent gas, NH
3Gas is as nitrogenous source.H
2Or N
2Or H
2And N
2Air-fuel mixture enleanment throughput 2500-3500sccm, NH
3Gas 500-7000sccm, the conversion zone temperature also can be 500-1050 ℃, growth time is can obtain the GaN film under the condition of 8-20min.V/III refers to the mol ratio of N and Ga, referring to subordinate list than being 500-3000.Gas flow control is controlled by mass flowmenter.
The present invention feeds carrier gas H
2, or N
2, also can be H
2, and N
2Mist; Ammonia and metal organic gallium source and metal organo indium source provide nitrogenous source, gallium source and indium source; By the control carrier gas, parameters such as gallium source and indium source gas flow, and growth time is controlled the thickness of film.
The method of mixing silicon or mixing magnesium of the preparation utilization routine of N type layer and P type layer GaN is finished.Ni/AuTi/Al is a metal electrode among Fig. 1.
Claims (5)
1, at β-Ga
2O
3The method of growing InGaN on the backing material/GaN quantum well LED device architecture is characterized in that the β-Ga to growing in the MOCVD system
2O
3Substrate carries out material heat treatment under 500-1050 ℃ of temperature, probable back feeds ammonia and carries out surfaces nitrided; Feed carrier gas N 500-1050 ℃ of temperature range
2, ammonia and metal organic source, by the control carrier gas, parameters such as source gas flow and growth temperature are at β-Ga
2O
3Synthetically grown low temperature GaN cushioning layer material on the substrate; With the MOCVD method at β-Ga
2O
3Under 500-1050 ℃ of temperature, mix Si growth N type GaN on the substrate behind the growing GaN cushioning layer material; With the MOCVD method at β-Ga
2O
3Then grow behind the growth N type GaN layer on the substrate and be respectively the GaN/InGaN multi-quantum pit structure in 5-10 the cycle of 15-20nm and 5-15nm respectively with 700-900 ℃ and the 600-800 ℃ bed thickness of growing; Reach 3*10 by Mg doped growing one deck doping content at last
17Cm
-1The LED device architecture of P type GaN layer; And to this structure in the activation of annealing of 600-800 ℃ of temperature and 0.1-1 hour annealing time.
2, by the method for the described growing InGaN of claim 1/GaN quantum well LED device architecture, it is characterized in that organic gallium source is trimethyl gallium and trimethyl indium, flow is respectively 1-50sccm and 50-200sccm, and growth temperature 500-1050 ℃, the time is 10-60 minute; NH
3Gas 500-700sccm, V/III refers to the mol ratio of N and Ga than being 500-3000.
3, by the method for claim 1 or 2 described growing InGaNs/GaN quantum well LED device architecture, it is characterized in that in the MOCVD system, at β-Ga
2O
3On the substrate, 500-1050 ℃ of temperature range synthetically grown concentration less than 1-10*10
16Cm
-1The GaN material.
4,, it is characterized in that growth one deck doping content is 1-10*10 on this GaN material by the method for claim 1 or 2 described growing InGaNs/GaN quantum well LED device architecture
18Cm
-1N type layer GaN.
5, by the method for claim 1 or 2 described growing InGaNs/GaN quantum well LED device architecture, it is characterized in that P type layer GaN, especially 3*10
17Cm
-1P type GaN.
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|---|---|---|---|
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|---|---|---|---|
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