CN103031595B - It is grown in LiGaO2Nonpolar doping GaN film on substrate and preparation method thereof - Google Patents
It is grown in LiGaO2Nonpolar doping GaN film on substrate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses and be grown in LiGaO2Doping GaN film on substrate, including the LiGaO being arranged in order from the bottom to top2Substrate, non-polar m-surface GaN cushion, non-polar m-surface GaN epitaxial layer, nonpolar doping GaN film；Described nonpolar GaN film is nonpolar p-type GaN film or nonpolar n-type GaN film。The preparation method that the invention also discloses above-mentioned nonpolar doping GaN film。Compared with prior art, it is simple that the present invention has growth technique, the advantage that preparation cost is cheap, and the nonpolar doping GaN film defect concentration of preparation is low, crystalline quality good, and electric property is good。
Description
Technical field
The present invention relates to nonpolar doping GaN film and preparation method thereof, particularly to being grown in LiGaO2Nonpolar doping GaN film on substrate and preparation method thereof。
Background technology
LED is referred to as forth generation lighting source or green light source, has the features such as energy-saving and environmental protection, life-span length, volume be little, it is possible to be widely used in the fields such as various general lighting, instruction, display, decoration, backlight and urban landscape。Currently, under the background that global warming problem is increasingly severe, save the energy, major issue faced by reduce greenhouse gas emission and become the whole world common。Low-carbon economy based on low energy consumption, low stain, low emission, will become the important directions of economic development。At lighting field, the application of LED luminous product is just attract the sight of common people, and LED is as a kind of novel green light source product, the necessarily trend of future development, and 21st century will be with the epoch of the LED novel illumination light source being representative。
III-nitride semiconductor material GaN manufactures the material that efficient LED devices is ideal。At present, the luminous efficiency of GaN base LED has reached 28% and also now in further growth, and this numerical value is significantly larger than the luminous efficiency of the lighting systems such as current normally used electric filament lamp (being about 2%) or fluorescent lamp (being about 10%)。Data statistics shows, the current electric consumption on lighting of China, every year more than 410,000,000,000 degree, exceedes Britain's whole nation power consumption of a year。If replacing whole electric filament lamp with LED or part replacing fluorescent lamp, the electric consumption on lighting close to half can be saved, exceed the generated energy that Three Gorges Projects are annual。Therefore the greenhouse gas emission produced because of illumination also can be substantially reduced。It addition, compared with fluorescent lamp, GaN base LED is without poisonous mercury element, and is about 100 times of this type of illuminations service life。
LED really to realize extensive extensive use, it is necessary to improves the luminous efficiency of LED chip further。Although the luminous efficiency of LED alreadys more than daylight lamp and electric filament lamp, but commercialization LED luminous efficiency is again below sodium vapor lamp (150lm/W), unit lumens/watt on the high side。At present, the luminous efficiency of LED chip is not high enough, and one is primarily due to what its Sapphire Substrate caused。There are two severe problems in the LED technology based on Sapphire Substrate。First, the mismatch ratio of sapphire and GaN lattice is up to 17%, and so high lattice mismatch makes the LED on sapphire have significantly high defect concentration, leverages the luminous efficiency of LED chip。Secondly, Sapphire Substrate price is sufficiently expensive so that nitride LED production cost significantly high (Sapphire Substrate occupies sizable ratio in the cost of manufacture of LED)。
The not high enough another one of the luminous efficiency of LED chip is primarily due to now widely used GaN base LED and has polarity。The ideal material of currently manufactured efficient LED devices is GaN。GaN is Patterns for Close-Packed Hexagonal Crystal structure, and its crystal face is divided into polar surface c face [(0001) face] and non-polar plane a face [(11-20) face] and m face [(1-100) face]。At present, to be all based on greatly the polar surface of GaN built-up for GaN base LED。On polar surface GaN, the barycenter of Ga atom set and atom N set is misaligned, thus forming electric dipole, produce spontaneous polarization field and piezoelectric polarization fields, and then cause quantum constraint Stark effect (Quant μm of-confinedStarkerEffect, QCSE), electronics is made to separate with hole, the radiation recombination efficiency of carrier reduces, and finally affects the luminous efficiency of LED, and causes the instability of LED emission wavelength。Solving this problem best bet is that the GaN material adopting non-polar plane makes LED, to eliminate the impact of quantum constraint Stark effect。Theoretical research shows, uses nonpolar face GaN to manufacture LED, and LED luminous efficiency can be made to improve nearly one times。
As can be seen here, LED will being made really to realize extensive extensive use, improve the luminous efficiency of LED chip, and reduce its manufacturing cost, one of the most basic way researches and develops the non-polar GaN-based LED epitaxial chip on Novel substrate exactly。And the n-type of nonpolar GaN film and p-type doping are the preconditions realizing non-polar GaN-based LED, therefore the n-type of Novel substrate Epitaxial growth nonpolar GaN film and p-type doping are always up focus and the difficult point of research。
Summary of the invention
In order to overcome disadvantages mentioned above and the deficiency of prior art, it is an object of the invention to provide one and be grown in LiGaO2Nonpolar doping GaN film on substrate, has crystal mass good, and doping content is high, the advantage that carrier mobility is high。Another object of the present invention is to the preparation method that above-mentioned nonpolar doping GaN film is provided。
The purpose of the present invention is achieved through the following technical solutions:
It is grown in LiGaO2Nonpolar doping GaN film on substrate, including the LiGaO being arranged in order from the bottom to top2Substrate, non-polar m-surface GaN cushion, non-polar m-surface GaN epitaxial layer, nonpolar doping GaN film；Described nonpolar GaN film is nonpolar p-type GaN film or nonpolar n-type GaN film。
Described LiGaO2The crystal orientation of substrate is 0.2 ~ 0.5 ° of (110) direction of (100) crystal face deflection。
The thickness of described non-polar m-surface GaN cushion is 30 ~ 60nm；The thickness of described non-polar m-surface GaN epitaxial layer is 150 ~ 250nm；The thickness of described nonpolar n-type doping GaN film is 100nm ~ 5 μm, and electron concentration is 1.0 × 1017~5.0×1019cm-3；The thickness of described p-type doping GaN film is 100nm ~ 5 μm；Hole concentration is 1.0 × 1016~2.0×1018cm-3。
It is grown in LiGaO2The preparation method of the nonpolar doping GaN film on substrate, comprises the following steps:
(1) LiGaO is chosen2Substrate, chooses crystal orientation；
(2) it is annealed substrate processing: substrate toasts after 3-5h air cooling at 900 ~ 1000 DEG C to room temperature；
(3) substrate is carried out surface cleaning process；
(4) adopting low temperature molecular beam epitaxy technique growing nonpolar m face GaN cushion, process conditions are: underlayer temperature is 220-350 DEG C, pass into Ga evaporation source and N plasma, and chamber pressure is 5 ~ 7 × 10-5Torr, the radio-frequency power producing plasma nitrogen are 200 ~ 300W, V/III than be 50 ~ 60, the speed of growth be 0.4 ~ 0.6ML/s；
(5) pulse laser deposition process growing nonpolar m face GaN epitaxial layer is adopted, process conditions are: underlayer temperature rises to 450 ~ 550 DEG C, adopt pulsed laser ablation Ga target, pass into N plasma simultaneously, radio-frequency power is 200 ~ 300W, and chamber pressure is 3 ~ 5 × 10-5Torr, laser energy is 120 ~ 180mJ, and frequency is 10 ~ 30Hz；
(6) pulse laser deposition process growing nonpolar doping GaN film is adopted, the process conditions of nonpolar p-type doping GaN film are: underlayer temperature is 450 ~ 550 DEG C, adopting pulsed laser ablation bombardment GaMg mixing target, pass into N plasma during growth, chamber pressure is 5 ~ 7 × 10-5Torr, radio-frequency power is 200 ~ 300W, and laser energy is 120 ~ 180mJ, and frequency is 10 ~ 30Hz；
The process conditions of nonpolar n-type doping GaN film are: underlayer temperature is 450 ~ 550 DEG C, adopts pulsed laser ablation GaSi mixing target, passes into N plasma during growth, and chamber pressure is 5 ~ 7 × 10-5Torr, radio-frequency power is 200 ~ 300W, and laser energy is 120 ~ 180mJ, and frequency is 10 ~ 30Hz。
Step (3) is described carries out surface cleaning process to substrate, particularly as follows: by LiGaO2Substrate puts in deionized water ultrasonic cleaning 5 ~ 10 minutes under room temperature, removes LiGaO2Substrate surface pickup granule, then sequentially pass through hydrochloric acid, acetone, washing with alcohol, remove surface organic matter；LiGaO after cleaning2Substrate dries up with high-purity drying nitrogen；Afterwards by LiGaO2Substrate puts into MBE growth at low temperature room, under UHV condition, underlayer temperature rises to 850 ~ 900 DEG C, toasts 20 ~ 30 minutes, removes LiGaO2The impurity that substrate surface is remaining。
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) present invention uses LiGaO2As substrate, adopt low temperature molecular beam epitaxy technology at LiGaO simultaneously2Substrate first grows one layer of non-polar m-surface GaN cushion, it is thus achieved that lattice mismatch very low between substrate and non-polar m-surface GaN epitaxial layer, be conducive to depositing the nonpolar GaN film of low defect, greatly improve the luminous efficiency of SQW。
(2) adopt low temperature molecular beam epitaxy technology at LiGaO2Substrate first grows one layer of non-polar m-surface GaN cushion, can guarantee that LiGaO at low temperatures2The stability of substrate, reduces the lattice mismatch that causes of volatilization of lithium ion and violent interfacial reaction, thus laying good basis for next step growing nonpolar m face GaN epitaxial layer。
(3) pulse laser deposition process is adopted to prepare nonpolar n or p-type doping GaN film, on non-polar plane, growth is conducive to doping, doping content can be improved, the mobility of carrier, the efficiency of nitride device such as semiconductor laser, light emitting diode and solaode can be increased substantially。
(4) LiGaO is used2As substrate, it is easy to obtain, low price, advantageously reduce production cost。
Accompanying drawing explanation
Fig. 1 be embodiment 1 preparation be grown in LiGaO2The schematic cross-section of the nonpolar n-type doping GaN film on substrate。
Fig. 2 be embodiment 1 preparation be grown in LiGaO2The XRD test figure of the nonpolar n-type doping GaN film on substrate。
Fig. 3 be embodiment 2 preparation be grown in LiGaO2The XRD test figure of the nonpolar p-type doping GaN film on substrate。
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this。
Embodiment 1
The present invention is grown in LiGaO2The preparation method of the doping GaN film on substrate, comprises the following steps:
(1) substrate and crystal orientation are chosen: adopt LiGaO2Substrate, crystal orientation is 0.2 ° of (110) direction of (100) crystal face deflection。
(2) be annealed substrate processing: by substrate at 900 DEG C after high-temperature baking 3h air cooling to room temperature。
(3) substrate is carried out surface cleaning process: by LiGaO2Substrate puts in deionized water ultrasonic cleaning 5 minutes under room temperature, removes LiGaO2Substrate surface pickup granule, then sequentially pass through hydrochloric acid, acetone, washing with alcohol, remove surface organic matter；LiGaO after cleaning2Substrate dries up with high-purity drying nitrogen；Afterwards by LiGaO2Substrate puts into MBE growth at low temperature room, under UHV condition, underlayer temperature rises to 850 DEG C, high-temperature baking 20 minutes, removes LiGaO2The impurity that substrate surface is remaining。
(4) adopting low temperature molecular beam epitaxy technique growing nonpolar m face GaN cushion, thickness is 30nm。Process conditions are: underlayer temperature is 220 DEG C, pass into Ga evaporation source and N plasma, and chamber pressure is 5 × 10-5Torr, the radio-frequency power producing plasma nitrogen are 200W, V/III than be 50, the speed of growth be 0.4ML/s。
(5) adopting pulse laser deposition process growing nonpolar m face GaN epitaxial layer, thickness is 150nm。Process conditions are: underlayer temperature rises to 450 DEG C, adopt pulsed laser ablation Ga target, pass into N plasma simultaneously, and radio-frequency power is 200W, and chamber pressure is 3 × 10-5Torr, laser energy are 120mJ, and frequency is 10Hz。
(6) adopting pulse laser deposition process growing nonpolar n-type doping GaN film, thickness is 100nm, and process conditions are: underlayer temperature is 450 DEG C, adopts pulsed laser ablation GaSi mixing target, passes into N plasma during growth, and chamber pressure is 5 × 10-5Torr, radio-frequency power is 200W, and laser energy is 120mJ, and frequency is 10Hz。
As it is shown in figure 1, the present embodiment prepare be grown in LiGaO2Nonpolar doping GaN film schematic diagram on substrate, including being grown in LiGaO2Non-polar m-surface GaN cushion 12 on substrate 11, is grown in the non-polar m-surface GaN epitaxial layer 13 on non-polar m-surface GaN cushion and the nonpolar n-type doping GaN film 14 being grown on non-polar GaN epitaxial layer。Wherein, the thickness of described non-polar m-surface GaN cushion is 30nm；The thickness of described non-polar m-surface GaN epitaxial layer is 150nm；The thickness of described nonpolar n-type doping GaN film is 100nm。
Fig. 2 be the present embodiment prepare be grown in LiGaO2The XRD test figure of the nonpolar n-type doping GaN film on substrate (100) face。Test obtains half-peak breadth (FWHM) value of n-type doping GaN film × ray swing curve, its half-peak breadth (FWHM) value is 0.0625 °, show no matter nonpolar n-type doping GaN film prepared by the present invention is in defect concentration or at crystalline quality, all has extraordinary performance。
Prepared by the present invention is grown in LiGaO2On substrate nonpolar n-type doping GaN film be room temperature Hall test result in temperature: temperature be under 293K Hall spectrum test obtain n-type doping GaN electron concentration be 5 × 1018cm-3, electron mobility is 300cm2/ v s, it was shown that nonpolar n-type doping GaN film prepared by the present invention has extraordinary performance。
Embodiment 2
The present invention is grown in LiGaO2The preparation method of the nonpolar doping GaN film on substrate, comprises the following steps:
(1) substrate and crystal orientation are chosen: adopt LiGaO2Substrate, crystal orientation is 0.5 ° of (110) direction of (100) crystal face deflection。
(2) be annealed substrate processing: by substrate at 1000 DEG C after high-temperature baking 5h air cooling to room temperature。
(3) substrate is carried out surface cleaning process: by LiGaO2Substrate puts in deionized water ultrasonic cleaning 10 minutes under room temperature, removes LiGaO2Substrate surface pickup granule, then sequentially pass through hydrochloric acid, acetone, washing with alcohol, remove surface organic matter；LiGaO after cleaning2Substrate dries up with high-purity drying nitrogen；Afterwards by LiGaO2Substrate puts into MBE growth at low temperature room, under UHV condition, underlayer temperature rises to 900 DEG C, high-temperature baking 30 minutes, removes LiGaO2The impurity that substrate surface is remaining。
(4) adopting low temperature molecular beam epitaxy technique growing nonpolar m face GaN cushion, thickness is 60nm。Process conditions are: underlayer temperature is 350 DEG C, pass into Ga evaporation source and N plasma, and chamber pressure is 7 × 10-5Torr, the radio-frequency power producing plasma nitrogen are 300W, V/III than be 60, the speed of growth be 0.6ML/s。
(5) adopting pulse laser deposition process growing nonpolar m face GaN epitaxial layer, thickness is 250nm。Process conditions are: underlayer temperature rises to 550 DEG C, adopt pulsed laser ablation Ga target, pass into N plasma simultaneously, and radio-frequency power is 300W, and chamber pressure is 5 × 10-5Torr, laser energy are 180mJ, and frequency is 30Hz。
(6) adopting pulse laser deposition process growth p-type doping GaN film, thickness is 100nm。Process conditions are: underlayer temperature is 450 DEG C, adopt pulsed laser ablation bombardment GaMg mixing target, pass into N plasma during growth, and chamber pressure is 5 × 10-5Torr, radio-frequency power is 200W, and laser energy is 120mJ, and frequency is 10Hz。
Prepared by the present embodiment is grown in LiGaO2Nonpolar p-type doping GaN film on substrate, including the LiGaO being arranged in order from the bottom to top2Substrate, non-polar m-surface GaN cushion, non-polar m-surface GaN epitaxial layer, nonpolar p-type doping GaN film；Wherein, the thickness of described non-polar m-surface GaN cushion is 60nm；The thickness of described non-polar m-surface GaN epitaxial layer is 250nm；The thickness of described nonpolar p-type doping GaN film is 100nm。
Fig. 3 be the present embodiment prepare be grown in LiGaO2The XRD test figure of the nonpolar p-type doping GaN film on substrate (100) face。Test obtains half-peak breadth (FWHM) value of p-type doping GaN film × ray swing curve, its half-peak breadth (FWHM) value is 0.0738 °, show no matter nonpolar p-type doping GaN film prepared by the present invention is in defect concentration or at crystalline quality, all has extraordinary performance。
Prepared by the present embodiment is grown in LiGaO2Non-polar m face n on substrate and p-type doping GaN film is room temperature Hall test result in temperature: be that under 293K, the test of Hall spectrum obtains the hole concentration of p-type doping GaN in temperature be 1 × 1017cm-3, hole mobility is 65cm2/ v s。Show that nonpolar p-type doping GaN film prepared by the present invention has extraordinary performance。
Embodiment 3
The present embodiment is except following characteristics, and all the other features are same with embodiment 1:
Step (6) is: adopt pulse laser deposition process growing nonpolar n-type doping GaN film, thickness is 5 μm, and process conditions are: underlayer temperature is 550 DEG C, adopts pulsed laser ablation GaSi mixing target, passing into N plasma during growth, chamber pressure is 7 × 10-5Torr, radio-frequency power is 300W, and laser energy is 180mJ, and frequency is 30Hz。
Embodiment 4
The present embodiment is except following characteristics, and all the other features are same with embodiment 2:
Step (6) is: adopting pulse laser deposition process growth p-type doping GaN film, thickness is 5 μm。Process conditions are: underlayer temperature is 550 DEG C, adopt pulsed laser ablation bombardment GaMg mixing target, pass into N plasma during growth, and chamber pressure is 7 × 10-5Torr, radio-frequency power is 300W, and laser energy is 180mJ, and frequency is 30Hz。
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted by the embodiments; the change made under other any spirit without departing from the present invention and principle, modification, replacement, combination, simplification; all should be the substitute mode of equivalence, be included within protection scope of the present invention。
Claims (2)
1. it is grown in LiGaO2The preparation method of the nonpolar doping GaN film on substrate, it is characterised in that comprise the following steps:
(1) LiGaO is chosen2Substrate, chooses crystal orientation；Described crystal orientation is 0.2～0.5 ° of (110) direction of (100) crystal face deflection；
(2) it is annealed substrate processing: substrate toasts after 3～5h air cooling at 900～1000 DEG C to room temperature；
(3) substrate is carried out surface cleaning process；
(4) adopting low temperature molecular beam epitaxy technique growing nonpolar m face GaN cushion, process conditions are: underlayer temperature is 220-350 DEG C, pass into Ga evaporation source and N plasma, and chamber pressure is 5～7 × 10-5Torr, the radio-frequency power producing plasma nitrogen are 200～300W, and V/III than being 0.4～0.6ML/s for 50-60, the speed of growth；The thickness of described non-polar m-surface GaN cushion is 30～60nm；
(5) pulse laser deposition process growing nonpolar m face GaN epitaxial layer is adopted, process conditions are: underlayer temperature rises to 450～550 DEG C, adopt pulsed laser ablation Ga target, pass into N plasma simultaneously, radio-frequency power is 200～300W, and chamber pressure is 3～5 × 10-5Torr, laser energy is 120-180mJ, and frequency is 10～30Hz；The thickness of described non-polar m-surface GaN epitaxial layer is 150～250nm；
(6) pulse laser deposition process growing nonpolar doping GaN film is adopted, the process conditions of nonpolar p-type doping GaN film are: underlayer temperature is 450～550 DEG C, adopting pulsed laser ablation bombardment GaMg mixing target, pass into N plasma during growth, chamber pressure is 5～7 × 10-5Torr, radio-frequency power is 200-300W, and laser energy is 120～180mJ, and frequency is 10～30Hz；The thickness of described p-type doping GaN film is 100nm～5 μm；Hole concentration is 1.0 × 1016～2.0 × 1018cm-3；
The process conditions of nonpolar n-type doping GaN film are: underlayer temperature is 450～550 DEG C, adopts pulsed laser ablation GaSi mixing target, passes into N plasma during growth, and chamber pressure is 5～7 × 10-5Torr, radio-frequency power is 200-300W, and laser energy is 120-180mJ, and frequency is 10～30Hz；The thickness of described nonpolar n-type doping GaN film is 100nm～5 μm, and electron concentration is 1.0 × 1017～5.0 × 1019cm-3。
2. according to claim 1 it is grown in LiGaO2The preparation method of the nonpolar doping GaN film on substrate, it is characterised in that step (3) is described carries out surface cleaning process to substrate, particularly as follows: by LiGaO2Substrate puts in deionized water ultrasonic cleaning 5～10 minutes under room temperature, removes LiGaO2Substrate surface pickup granule, then sequentially pass through hydrochloric acid, acetone, washing with alcohol, remove surface organic matter；LiGaO after cleaning2Substrate dries up with high-purity drying nitrogen；Afterwards by LiGaO2Substrate puts into MBE growth at low temperature room, under UHV condition, underlayer temperature rises to 850～900 DEG C, toasts 20～30 minutes, removes LiGaO2The impurity that substrate surface is remaining。
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| 脉冲激光沉积系统（PLD）的应用-制备GaN薄膜;李晓兰等;《现代电子技术》;20081115(第22期);第12-14页 * |
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