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CN203085627U - Non-polar blue LED epitaxial wafer grown on LiGaO2 substrate - Google Patents

Non-polar blue LED epitaxial wafer grown on LiGaO2 substrate Download PDF

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CN203085627U
CN203085627U CN 201220684170 CN201220684170U CN203085627U CN 203085627 U CN203085627 U CN 203085627U CN 201220684170 CN201220684170 CN 201220684170 CN 201220684170 U CN201220684170 U CN 201220684170U CN 203085627 U CN203085627 U CN 203085627U
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李国强
杨慧
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South China University of Technology SCUT
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Abstract

The utility model discloses a non-polar blue light LED epitaxial wafer growing on a LiGaO2 substrate comprising, from bottom to top, a LiGao2 substrate, a non-polar m surface GaN buffer layer, a non-polar m surface GaN epitaxial layer, a non-polar non-doped GaN layer, a non-polar n-type doped GaN film, a non-polar InGaN/Gan quantum well layer, and a non-polar p-type doped GaN film sequentially. Compared to the prior art, the utility model is advantageous in that the growing technology is simple, the preparation costs are low; the prepared non-polar blue light LED epitaxial wafer has advantages of low defect density, good crystallization quality, and good electrical, optical properties.

Description

生长在LiGaO2衬底上的非极性蓝光LED外延片Non-polar blue LED epitaxial wafer grown on LiGaO2 substrate

技术领域technical field

本实用新型涉及非极性蓝光LED外延片,特别涉及生长在LiGaO2衬底上的非极性蓝光LED外延片。The utility model relates to a nonpolar blue light LED epitaxial sheet, in particular to a nonpolar blue light LED epitaxial sheet grown on a LiGaO2 substrate.

背景技术Background technique

LED被称为第四代照明光源或绿色光源,具有节能、环保、寿命长、体积小等特点,可以广泛应用于各种普通照明、指示、显示、装饰、背光源、和城市夜景等领域。当前,在全球气候变暖问题日趋严峻的背景下,节约能源、减少温室气体排放成为全球共同面对的重要问题。以低能耗、低污染、低排放为基础的低碳经济,将成为经济发展的重要方向。在照明领域,LED发光产品的应用正吸引着世人的目光,LED作为一种新型的绿色光源产品,必然是未来发展的趋势,二十一世纪将是以LED为代表的新型照明光源的时代。LED is called the fourth-generation lighting source or green light source. It has the characteristics of energy saving, environmental protection, long life, and small size. It can be widely used in various fields such as general lighting, indication, display, decoration, backlight, and urban night scenes. At present, under the background of the increasingly serious problem of global warming, energy conservation and reduction of greenhouse gas emissions have become important issues faced by the whole world. A low-carbon economy based on low energy consumption, low pollution, and low emissions will become an important direction of economic development. In the field of lighting, the application of LED light-emitting products is attracting the attention of the world. As a new type of green light source product, LED must be the trend of future development. The 21st century will be an era of new lighting sources represented by LEDs.

III族氮化物半导体材料GaN是制造高效LED器件最为理想的材料。目前,GaN基LED的发光效率现在已经达到28%并且还在进一步的增长,该数值远远高于目前通常使用的白炽灯(约为2%)或荧光灯(约为10%)等照明方式的发光效率。数据统计表明,我国目前的照明用电每年在4100亿度以上,超过英国全国一年的用电量。如果用LED取代全部白炽灯或部分取代荧光灯,可节省接近一半的照明用电,超过三峡工程全年的发电量。因照明而产生的温室气体排放也会因此而大大降低。另外,与荧光灯相比,GaN基LED不含有毒的汞元素,且使用寿命约为此类照明工具的100倍。Group III nitride semiconductor material GaN is the most ideal material for manufacturing high-efficiency LED devices. At present, the luminous efficiency of GaN-based LEDs has reached 28% and is still increasing, which is much higher than that of the commonly used incandescent lamps (about 2%) or fluorescent lamps (about 10%). Luminous efficiency. Statistics show that my country's current lighting electricity consumption is more than 410 billion kWh per year, which exceeds the annual electricity consumption of the UK. If LEDs are used to replace all incandescent lamps or partially replace fluorescent lamps, nearly half of the lighting power consumption can be saved, exceeding the annual power generation of the Three Gorges Project. Greenhouse gas emissions from lighting are also significantly reduced as a result. In addition, compared with fluorescent lamps, GaN-based LEDs do not contain toxic mercury elements, and the service life is about 100 times longer than that of such lighting tools.

LED要真正实现大规模广泛应用,需要进一步提高LED芯片的发光效率。虽然LED的发光效率已经超过日光灯和白炽灯,但是商业化LED发光效率还是低于钠灯(150lm/W),单位流明/瓦的价格偏高。目前,LED芯片的发光效率不够高,一个主要原因是由于其蓝宝石衬底造成的。基于蓝宝石衬底的LED技术存在两个严峻的问题。首先,蓝宝石与GaN晶格的失配率高达17%,如此高的晶格失配使得蓝宝石上的LED外延片有很高的缺陷密度,大大影响了LED芯片的发光效率。其次,蓝宝石衬底价格十分昂贵,使得氮化物LED生产成本很高(蓝宝石衬底在LED的制作成本中占有相当大的比例)。If LEDs are to be widely used on a large scale, it is necessary to further improve the luminous efficiency of LED chips. Although the luminous efficiency of LED has surpassed that of fluorescent lamps and incandescent lamps, the luminous efficiency of commercial LEDs is still lower than that of sodium lamps (150lm/W), and the price per lumen/watt is relatively high. At present, the luminous efficiency of LED chips is not high enough, one of the main reasons is due to its sapphire substrate. LED technology based on sapphire substrates has two serious problems. First of all, the lattice mismatch rate between sapphire and GaN is as high as 17%. Such a high lattice mismatch makes the LED epitaxial wafer on sapphire have a high defect density, which greatly affects the luminous efficiency of the LED chip. Secondly, the sapphire substrate is very expensive, which makes the production cost of nitride LEDs very high (the sapphire substrate occupies a considerable proportion in the production cost of LEDs).

LED芯片的发光效率不够高的另外一个主要原因是由于目前广泛使用的GaN基LED具有极性。目前制造高效LED器件最为理想的材料是GaN。GaN为密排六方晶体结构,其晶面分为极性面c面[(0001)面]和非极性面a面[(11-20)面]及m面[(1-100)面]。目前,GaN基LED大都基于GaN的极性面构建而成。在极性面GaN上,Ga原子集合和N原子集合的质心不重合,从而形成电偶极子,产生自发极化场和压电极化场,进而引起量子束缚斯塔克效应(Quantum-confined Starker Effect,QCSE),使电子和空穴分离,载流子的辐射复合效率降低,最终影响LED的发光效率,并造成LED发光波长的不稳定。解决这一问题最好的办法是采用非极性面的GaN材料制作LED,以消除量子束缚斯塔克效应的影响。理论研究表明,使用非极性面GaN来制造LED,将可使LED发光效率提高近一倍。Another main reason why the luminous efficiency of LED chips is not high enough is that GaN-based LEDs widely used at present have polarity. At present, the most ideal material for manufacturing high-efficiency LED devices is GaN. GaN has a close-packed hexagonal crystal structure, and its crystal planes are divided into polar c-plane [(0001) plane], non-polar a-plane [(11-20) plane] and m-plane [(1-100) plane] . At present, GaN-based LEDs are mostly constructed based on the polar face of GaN. On the polar plane GaN, the centroids of the Ga atom assembly and the N atom assembly do not coincide, thereby forming an electric dipole, generating a spontaneous polarization field and a piezoelectric polarization field, and then causing the Quantum-confined Stark effect (Quantum-confined Stark effect). Starker Effect, QCSE), which separates electrons and holes, and reduces the radiative recombination efficiency of carriers, which ultimately affects the luminous efficiency of the LED and causes the instability of the LED luminous wavelength. The best way to solve this problem is to use non-polar GaN material to make LEDs to eliminate the influence of the quantum-bound Stark effect. Theoretical studies have shown that the use of non-polar surface GaN to manufacture LEDs will nearly double the luminous efficiency of LEDs.

由此可见,要使LED真正实现大规模广泛应用,提高LED芯片的发光效率,并降低其制造成本,最根本的办法就是研发新型衬底上的非极性GaN基LED外延芯片。因此新型衬底上外延生长非极性氮化镓LED外延片一直是研究的热点和难点。It can be seen that the most fundamental way to make LEDs truly realize large-scale and wide application, improve the luminous efficiency of LED chips, and reduce their manufacturing costs is to develop non-polar GaN-based LED epitaxial chips on new substrates. Therefore, the epitaxial growth of non-polar gallium nitride LED epitaxial wafers on new substrates has always been a hot and difficult research point.

实用新型内容Utility model content

为了克服现有技术的上述缺点与不足,本实用新型的目的在于提供一种生长在LiGaO2衬底上的非极性蓝光LED外延片,具有缺陷密度低、结晶质量好,发光性能好的优点,且制备成本低廉。In order to overcome the above-mentioned shortcomings and deficiencies of the prior art, the purpose of this utility model is to provide a non-polar blue LED epitaxial wafer grown on a LiGaO2 substrate, which has the advantages of low defect density, good crystal quality and good luminous performance , and the preparation cost is low.

本实用新型的目的通过以下技术方案实现:The purpose of this utility model is achieved through the following technical solutions:

生长在LiGaO2衬底上的非极性蓝光LED外延片,包括由下至上依次排列的LiGaO2衬底、非极性m面GaN缓冲层、非极性m面GaN外延层、非极性非掺杂u-GaN层、非极性n型掺杂GaN薄膜、非极性InGaN/GaN量子阱层、非极性p型掺杂GaN薄膜。Nonpolar blue LED epitaxial wafer grown on LiGaO2 substrate, including LiGaO2 substrate, nonpolar m-plane GaN buffer layer, nonpolar m-plane GaN epitaxial layer, nonpolar nonpolar Doped u-GaN layer, non-polar n-type doped GaN film, non-polar InGaN/GaN quantum well layer, non-polar p-type doped GaN film.

所述LiGaO2衬底的晶体取向为(100)晶面偏向(110)方向0.2~0.5°。The crystal orientation of the LiGaO 2 substrate is that the (100) crystal plane is deflected to the (110) direction by 0.2-0.5°.

生长在LiGaO2衬底上的非极性蓝光LED外延片,所述非极性m面GaN缓冲层的厚度为30~60nm;所述非极性m面GaN外延层的厚度为150~250nm;非极性非掺杂u-GaN层的厚度为300~500nm;所述非极性n型掺杂GaN层的厚度为3~5μm;所述非极性InGaN/GaN量子阱层为5~10个周期的InGaN阱层/GaN垒层,其中InGaN阱层的厚度为2~3nm;GaN垒层的厚度为10~13nm;所述非极性p型掺杂GaN薄膜的厚度为350~500nm,所述非极性n型掺杂GaN薄膜的电子浓度为1.0×1017~5.0×1019cm-3,所述非极性p型掺杂GaN薄膜的空穴浓度为1.0×1016~2.0×1018cm-3A non-polar blue LED epitaxial wafer grown on a LiGaO 2 substrate, the thickness of the non-polar m-plane GaN buffer layer is 30-60 nm; the thickness of the non-polar m-plane GaN epitaxial layer is 150-250 nm; The thickness of the non-polar non-doped u-GaN layer is 300-500 nm; the thickness of the non-polar n-type doped GaN layer is 3-5 μm; the non-polar InGaN/GaN quantum well layer is 5-10 nm. A period of InGaN well layer/GaN barrier layer, wherein the thickness of the InGaN well layer is 2~3nm; the thickness of the GaN barrier layer is 10~13nm; the thickness of the nonpolar p-type doped GaN film is 350~500nm, The electron concentration of the non-polar n-type doped GaN film is 1.0×10 17 ~5.0×10 19 cm -3 , and the hole concentration of the non-polar p-type doped GaN film is 1.0×10 16 ~2.0 ×10 18 cm -3 .

生长在LiGaO2衬底上的非极性蓝光LED外延片的制备方法,包括以下步骤:The preparation method of the nonpolar blue light LED epitaxial wafer grown on the LiGaO2 substrate comprises the following steps:

(1)采用LiGaO2衬底,选取晶体取向;(1) Using LiGaO 2 substrate, select the crystal orientation;

(2)对衬底进行退火处理:将衬底在900~1000℃下烘烤3~5h后空冷至室温;(2) Annealing the substrate: bake the substrate at 900-1000°C for 3-5 hours, then air-cool to room temperature;

(3)对衬底进行表面清洁处理;(3) Surface cleaning of the substrate;

(4)采用低温分子束外延工艺生长非极性m面GaN缓冲层,工艺条件为:衬底温度为220~350℃,通入Ga蒸发源与N等离子体,反应室压力为5~7×10-5torr、产生等离子体氮的射频功率为200~300W,Ⅴ/Ⅲ比为50~60、生长速度为0.4~0.6ML/s;(4) Low-temperature molecular beam epitaxy is used to grow the non-polar m-plane GaN buffer layer. The process conditions are: the substrate temperature is 220-350°C, the Ga evaporation source and N plasma are introduced, and the reaction chamber pressure is 5-7× 10 -5 torr, the RF power for generating plasma nitrogen is 200~300W, the V/III ratio is 50~60, and the growth rate is 0.4~0.6ML/s;

(5)采用脉冲激光沉积工艺生长非极性m面GaN外延层,工艺条件为:衬底温度升至450~550℃,采用脉冲激光轰击Ga靶材,同时通入N2,反应室压力为3~5×10-5torr、激光能量为120~180mJ,激光频率为10~30Hz;(5) The non-polar m-plane GaN epitaxial layer is grown by pulsed laser deposition process. The process conditions are as follows: the substrate temperature rises to 450~550°C, pulsed laser is used to bombard the Ga target, and N 2 is introduced at the same time, and the reaction chamber pressure is 3~5×10 -5 torr, laser energy 120~180mJ, laser frequency 10~30Hz;

(6)采用分子束外延工艺生长非极性非掺杂u-GaN层,工艺条件为:衬底温度为700~800℃,通入Ga蒸发源与N等离子体,反应室压力为5~7×10-5torr、产生等离子体氮的射频功率为200~300W;(6) Molecular beam epitaxy is used to grow non-polar and non-doped u-GaN layers. The process conditions are: the substrate temperature is 700~800°C, the Ga evaporation source and N plasma are introduced, and the reaction chamber pressure is 5~7 ×10 -5 torr, the RF power for generating plasma nitrogen is 200~300W;

(7)采用脉冲激光沉积工艺生长非极性n型掺杂GaN薄膜,工艺条件为:衬底温度为450~550℃,采用脉冲激光轰击GaSi混合靶材,生长时通入N等离子体,反应室压力为5~7×10-5torr、射频功率为200~300W,激光能量为120~180mJ,激光频率为10~30Hz,电子载流子浓度由GaSi混合靶材中两种元素的原子比来控制,掺杂电子浓度1.0×1017~5.0×1019cm-3(7) The non-polar n-type doped GaN film is grown by pulsed laser deposition process. The process conditions are as follows: the substrate temperature is 450~550°C, the pulsed laser is used to bombard the GaSi mixed target, N plasma is introduced during the growth, and the reaction The chamber pressure is 5~7×10 -5 torr, the RF power is 200~300W, the laser energy is 120~180mJ, the laser frequency is 10~30Hz, and the electron carrier concentration is determined by the atomic ratio of the two elements in the GaSi mixed target To control, the doping electron concentration is 1.0×10 17 ~5.0×10 19 cm -3 ;

(8)采用分子束外延工艺生长非极性InGaN/GaN量子阱,工艺条件为:衬底温度为500~750℃,通入Ga蒸发源与N等离子体,反应室压力为5~7×10-5torr,产生等离子体氮的射频功率为200~300W;(8) Molecular beam epitaxy is used to grow non-polar InGaN/GaN quantum wells. The process conditions are: the substrate temperature is 500~750°C, the Ga evaporation source and N plasma are introduced, and the reaction chamber pressure is 5~7×10 -5 torr, the RF power for generating plasma nitrogen is 200~300W;

(9)采用脉冲激光沉积工艺生长非极性p型掺杂GaN薄膜,工艺条件为:衬底温度为450~550℃,采用脉冲激光轰击GaMg混合靶材来生长p型GaN薄膜,生长时通入N等离子体,反应室压力为5~7×10-5torr,射频功率为200~300W,激光能量为120~180mJ,激光频率为10~30Hz,空穴的载流子浓由GaMg混合靶材中两种元素的原子比来控制,掺杂空穴浓度1.0×1016~2.0×1018cm-3(9) The non-polar p-type doped GaN film is grown by pulsed laser deposition process. The process conditions are as follows: the substrate temperature is 450~550°C, and the pulsed laser is used to bombard the GaMg mixed target to grow the p-type GaN film. N plasma is injected, the pressure of the reaction chamber is 5~7×10 -5 torr, the radio frequency power is 200~300W, the laser energy is 120~180mJ, the laser frequency is 10~30Hz, and the carrier concentration of holes is obtained by GaMg mixed target The atomic ratio of the two elements in the material is controlled, and the doping hole concentration is 1.0×10 16 ~2.0×10 18 cm -3 .

生长在LiGaO2衬底上的非极性蓝光LED外延片的制备方法,包括所述非极性m面GaN缓冲层的厚度为30~60nm;所述非极性m面GaN外延层的厚度为150~250nm;非极性非掺杂u-GaN层的厚度为300~500nm;所述非极性n型掺杂GaN层的厚度为3~5μm;所述非极性InGaN/GaN量子阱层为5~10个周期的InGaN阱层/GaN垒层,其中InGaN阱层的厚度为2~3nm;GaN垒层的厚度为10~13nm;所述非极性p型掺杂GaN薄膜的厚度为350~500nm。The preparation method of the nonpolar blue LED epitaxial wafer grown on the LiGaO2 substrate, comprising the thickness of the nonpolar m-plane GaN buffer layer is 30 ~ 60nm; the thickness of the nonpolar m-plane GaN epitaxial layer is 150~250nm; the thickness of the nonpolar non-doped u-GaN layer is 300~500nm; the thickness of the nonpolar n-type doped GaN layer is 3~5μm; the nonpolar InGaN/GaN quantum well layer InGaN well layer/GaN barrier layer of 5-10 periods, wherein the thickness of the InGaN well layer is 2-3nm; the thickness of the GaN barrier layer is 10-13nm; the thickness of the non-polar p-type doped GaN film is 350~500nm.

生长在LiGaO2衬底上的非极性蓝光LED外延片的制备方法,步骤(3)所述对衬底进行表面清洁处理,具体为:The preparation method of the non-polar blue light LED epitaxial wafer grown on the LiGaO 2 substrate, the surface cleaning treatment of the substrate as described in step (3), specifically:

将LiGaO2衬底放入去离子水中室温下超声清洗5~10分钟,去除LiGaO2衬底表面粘污颗粒,再依次经过盐酸、丙酮、乙醇洗涤,去除表面有机物;清洗后的LiGaO2衬底用高纯干燥氮气吹干;之后将LiGaO2衬底放入低温分子束外延生长室,在超高真空条件下,将衬底温度升至850~900℃,烘烤20~30分钟,除去LiGaO2衬底表面残余的杂质。Put the LiGaO 2 substrate in deionized water and ultrasonically clean it at room temperature for 5 to 10 minutes to remove the dirt particles on the surface of the LiGaO 2 substrate, and then wash it with hydrochloric acid, acetone, and ethanol in order to remove the surface organic matter; the cleaned LiGaO 2 substrate Blow dry with high-purity dry nitrogen; then put the LiGaO 2 substrate into a low-temperature molecular beam epitaxy growth chamber, raise the substrate temperature to 850-900°C under ultra-high vacuum conditions, and bake for 20-30 minutes to remove LiGaO 2 Residual impurities on the surface of the substrate.

与现有技术相比,本实用新型具有以下优点和有益效果:Compared with the prior art, the utility model has the following advantages and beneficial effects:

(1)本实用新型使用LiGaO2作为衬底,同时采用低温分子束外延技术在LiGaO2衬底上先生长一层非极性m面GaN缓冲层,获得衬底与非极性m面GaN外延层之间很低的晶格失配度,有利于沉积低缺陷的非极性GaN薄膜,极大的提高了LED的发光效率。(1) This utility model uses LiGaO 2 as the substrate, and at the same time adopts low-temperature molecular beam epitaxy technology to grow a non-polar m-plane GaN buffer layer on the LiGaO 2 substrate to obtain the substrate and non-polar m-plane GaN epitaxy The very low lattice mismatch between layers is conducive to the deposition of low-defect non-polar GaN thin films, which greatly improves the luminous efficiency of LEDs.

(2)本实用新型采用低温分子束外延技术在LiGaO2衬底上先生长一层非极性m面GaN缓冲层,在低温下能保证LiGaO2衬底的稳定性,减少锂离子的挥发造成的晶格失配和剧烈界面反应,从而为下一步生长非极性m面GaN外延层打下良好基础。(2) The utility model adopts low-temperature molecular beam epitaxy technology to grow a layer of non-polar m-plane GaN buffer layer on the LiGaO 2 substrate, which can ensure the stability of the LiGaO 2 substrate at low temperature and reduce the volatilization of lithium ions. The lattice mismatch and severe interfacial reaction lay a good foundation for the next step of growing non-polar m-plane GaN epitaxial layer.

(3)本实用新型采用分子束外延与脉冲激光沉积工艺结合的办法制备出高质量非极性蓝光LED外延片,消除了极性面GaN带来的量子束缚斯塔克效应,提高了载流子的辐射复合效率,可大幅度提高氮化物器件如半导体激光器、发光二极管及太阳能电池的效率。(3) The utility model adopts the combination of molecular beam epitaxy and pulsed laser deposition technology to prepare high-quality non-polar blue LED epitaxial wafers, which eliminates the quantum-bound Stark effect brought about by GaN on the polar surface, and improves the current carrying capacity. The radiative recombination efficiency of electrons can greatly improve the efficiency of nitride devices such as semiconductor lasers, light-emitting diodes and solar cells.

(4)本实用新型使用LiGaO2作为衬底,容易获得,价格便宜,有利于降低生产成本。(4) The utility model uses LiGaO 2 as the substrate, which is easy to obtain and cheap, and is conducive to reducing production costs.

附图说明Description of drawings

图1为实施例1制备的生长在LiGaO2衬底上的非极性蓝光LED外延片的截面示意图。1 is a schematic cross-sectional view of a non-polar blue LED epitaxial wafer grown on a LiGaO 2 substrate prepared in Example 1.

图2为实施例1制备的生长在LiGaO2衬底上的非极性蓝光LED外延片的XRD测试图。2 is an XRD test chart of the non-polar blue LED epitaxial wafer grown on the LiGaO 2 substrate prepared in Example 1.

图3为实施例1制备的生长在LiGaO2衬底上的非极性蓝光LED外延片的光致发光PL谱测试图。3 is a photoluminescence PL spectrum test chart of the non-polar blue LED epitaxial wafer grown on the LiGaO 2 substrate prepared in Example 1.

图4为实施例1制备的生长在LiGaO2衬底上的非极性蓝光LED外延片的电致发光EL谱测试图。4 is an electroluminescence EL spectrum test diagram of the non-polar blue LED epitaxial wafer grown on the LiGaO 2 substrate prepared in Example 1.

具体实施方式Detailed ways

下面结合实施例及附图,对本实用新型作进一步地详细说明,但本实用新型的实施方式不限于此。The utility model will be described in further detail below in conjunction with the embodiments and accompanying drawings, but the implementation of the utility model is not limited thereto.

实施例1Example 1

本实施例生长在LiGaO2衬底上的非极性蓝光LED外延片的制备方法,包括以下步骤:The preparation method of the non-polar blue light LED epitaxial wafer grown on the LiGaO2 substrate in this embodiment comprises the following steps:

(1)采用LiGaO2衬底,选取晶体取向为(100)晶面偏向(110)方向0.2°;(1) Using LiGaO 2 substrate, the crystal orientation is selected as (100) crystal plane biased to (110) direction by 0.2°;

(2)对衬底进行退火处理:将衬底在900℃下高温烘烤3h后空冷至室温;(2) Anneal the substrate: bake the substrate at 900°C for 3 hours, then air cool to room temperature;

(3)对衬底进行表面清洁处理:将LiGaO2衬底放入去离子水中室温下超声清洗5分钟,去除LiGaO2衬底表面粘污颗粒,再依次经过盐酸、丙酮、乙醇洗涤,去除表面有机物;清洗后的LiGaO2衬底用高纯干燥氮气吹干;之后将LiGaO2衬底放入低温分子束外延生长室,在超高真空条件下,将衬底温度升至850℃,烘烤20分钟,除去LiGaO2衬底表面残余的杂质;(3) Clean the surface of the substrate: put the LiGaO 2 substrate in deionized water and ultrasonically clean it for 5 minutes at room temperature to remove the sticky particles on the surface of the LiGaO 2 substrate, and then wash with hydrochloric acid, acetone, and ethanol in sequence to remove the surface organic matter; the cleaned LiGaO 2 substrate is dried with high-purity dry nitrogen; then the LiGaO 2 substrate is placed in a low-temperature molecular beam epitaxy growth chamber, and the substrate temperature is raised to 850°C under ultra-high vacuum conditions, and baked 20 minutes, remove LiGaO 2 residual impurities on the substrate surface;

(4)采用低温分子束外延工艺生长非极性m面GaN缓冲层,工艺条件为:衬底温度为220℃,通入Ga蒸发源与N等离子体,反应室压力为5×10-5torr、产生等离子体氮的射频功率为200W,Ⅴ/Ⅲ比为50,生长速度为0.4ML/s;(4) The non-polar m-plane GaN buffer layer is grown by low-temperature molecular beam epitaxy. The process conditions are: the substrate temperature is 220°C, the Ga evaporation source and N plasma are introduced, and the reaction chamber pressure is 5×10 -5 torr , The radio frequency power for generating plasma nitrogen is 200W, the V/III ratio is 50, and the growth rate is 0.4ML/s;

(5)采用脉冲激光沉积工艺生长非极性m面GaN外延层,工艺条件为:衬底温度升至450℃,采用脉冲激光轰击Ga靶材,同时通入N2,反应室压力为3×10-5torr、激光能量为120mJ,激光频率为10Hz;(5) The non-polar m-plane GaN epitaxial layer was grown by pulsed laser deposition process. The process conditions were as follows: the substrate temperature was raised to 450°C, the pulsed laser was used to bombard the Ga target, and N 2 was introduced at the same time, and the pressure of the reaction chamber was 3× 10 -5 torr, laser energy 120mJ, laser frequency 10Hz;

(6)采用分子束外延工艺生长非极性非掺杂u-GaN层,工艺条件为:衬底温度为700℃,通入Ga蒸发源与N等离子体,反应室压力为5×10-5torr、产生等离子体氮的射频功率为200W;(6) Molecular beam epitaxy is used to grow non-polar and non-doped u-GaN layers. The process conditions are: the substrate temperature is 700°C, the Ga evaporation source and N plasma are introduced, and the reaction chamber pressure is 5×10 -5 torr, the RF power for generating plasma nitrogen is 200W;

(7)采用脉冲激光沉积工艺生长非极性n型掺杂GaN薄膜,工艺条件为:衬底温度为450℃,采用脉冲激光轰击GaSi混合靶材,生长时通入N等离子体,反应室压力为5×10-5torr、射频功率为200W,激光能量为120mJ,激光频率为10Hz,掺杂电子浓度1.0×1017cm-3(7) The non-polar n-type doped GaN film is grown by pulsed laser deposition process. The process conditions are as follows: the substrate temperature is 450°C, the pulsed laser is used to bombard the GaSi mixed target, N plasma is introduced during the growth, and the pressure of the reaction chamber is 5×10 -5 torr, RF power 200W, laser energy 120mJ, laser frequency 10Hz, doped electron concentration 1.0×10 17 cm -3 ;

(8)采用分子束外延工艺生长非极性InGaN/GaN量子阱,工艺条件为:衬底温度为500℃,通入Ga蒸发源与N等离子体,反应室压力为5×10-5torr、产生等离子体氮的射频功率为200W;(8) Nonpolar InGaN/GaN quantum wells are grown by molecular beam epitaxy. The process conditions are as follows: the substrate temperature is 500°C, the Ga evaporation source and N plasma are introduced, and the reaction chamber pressure is 5×10 -5 torr, The RF power for generating plasma nitrogen is 200W;

(9)采用脉冲激光沉积工艺生长非极性p型掺杂GaN薄膜,工艺条件为:衬底温度为450℃,采用脉冲激光轰击GaMg混合靶材来生长p型GaN薄膜,生长时通入N等离子体,反应室压力为5×10-5torr,射频功率为200-300W,激光能量为120mJ,激光频率为10Hz,空穴载流子浓度由GaMg混合靶材中两种元素的原子比来控制,掺杂空穴浓度1.0×1016cm-3(9) The non-polar p-type doped GaN film is grown by pulsed laser deposition process. The process conditions are as follows: the substrate temperature is 450°C, the pulsed laser is used to bombard the GaMg mixed target to grow the p-type GaN film, and N Plasma, the reaction chamber pressure is 5×10 -5 torr, the RF power is 200-300W, the laser energy is 120mJ, the laser frequency is 10Hz, and the hole carrier concentration is determined by the atomic ratio of the two elements in the GaMg mixed target control, the doping hole concentration is 1.0×10 16 cm -3 .

如图1所示,本实施例制备的生长在LiGaO2衬底上的非极性蓝光LED外延片,包括由下至上依次排列的LiGaO2衬底11、非极性m面GaN缓冲层12、非极性m面GaN外延层13、非极性非掺杂u-GaN层14、非极性n型掺杂GaN薄膜15、非极性InGaN/GaN量子阱层16、非极性p型掺杂GaN薄膜17;其中,所述非极性m面GaN缓冲层的厚度为30~60nm;所述非极性m面GaN外延层的厚度为150nm;非极性非掺杂u-GaN层的厚度为300nm;所述非极性n型掺杂GaN层的厚度为3μm;所述非极性InGaN/GaN量子阱层为5个周期的InGaN阱层/GaN垒层,其中InGaN阱层的厚度为2nm;GaN垒层的厚度为10nm;所述非极性p型掺杂GaN薄膜的厚度为350nm。As shown in Figure 1, the nonpolar blue LED epitaxial wafer grown on the LiGaO2 substrate prepared in this embodiment includes a LiGaO2 substrate 11, a nonpolar m-plane GaN buffer layer 12, Nonpolar m-plane GaN epitaxial layer 13, nonpolar non-doped u-GaN layer 14, nonpolar n-type doped GaN film 15, nonpolar InGaN/GaN quantum well layer 16, nonpolar p-type doped Doped GaN thin film 17; wherein, the thickness of the nonpolar m-plane GaN buffer layer is 30~60nm; the thickness of the nonpolar m-plane GaN epitaxial layer is 150nm; the thickness of the nonpolar non-doped u-GaN layer The thickness is 300nm; the thickness of the non-polar n-type doped GaN layer is 3 μm; the non-polar InGaN/GaN quantum well layer is 5 cycles of InGaN well layer/GaN barrier layer, wherein the thickness of the InGaN well layer is The thickness of the GaN barrier layer is 10 nm; the thickness of the non-polar p-type doped GaN film is 350 nm.

图2为本实施例制备的生长在LiGaO2衬底(100)面上的非极性蓝光LED外延片的XRD测试图。测试得到LED外延片×射线回摆曲线的半峰宽(FWHM)值,其半峰宽(FWHM)值低于0.1°。测试得到蓝光LED外延片卫星峰,其最强峰为GaN,左右旁边依次为量子阱的第一级卫星峰,第二级卫星峰,...表明本实用新型制备的非极性蓝光LED外延片无论是在缺陷密度还是在结晶质量,都具有非常好的性能。Fig. 2 is an XRD test pattern of the non-polar blue LED epitaxial wafer grown on the LiGaO 2 substrate (100) surface prepared in this embodiment. The half-maximum width (FWHM) value of the LED epitaxial wafer × ray hysteresis curve was obtained through the test, and its half-maximum width (FWHM) value was lower than 0.1°. The satellite peaks of the blue LED epitaxial wafers were tested, and the strongest peak was GaN, and the left and right sides were the first-level satellite peaks and the second-level satellite peaks of the quantum well. The flakes have very good properties both in terms of defect density and crystalline quality.

图3为本实施例制备的生长在LiGaO2衬底上的非极性m面蓝光LED外延片的在温度为室温下PL谱测试图。由图可知,温度为293K下PL谱测试得到发光峰波长为444nm,半峰宽为26nm,而且LED的厚度为5.95um。表明本实用新型制备的非极性GaN薄膜在光学性质上具有非常好的性能。Fig. 3 is a PL spectrum test chart of the non-polar m-plane blue LED epitaxial wafer grown on the LiGaO 2 substrate prepared in this embodiment at room temperature. It can be seen from the figure that the PL spectrum test under the temperature of 293K shows that the luminous peak wavelength is 444nm, the half-maximum width is 26nm, and the thickness of the LED is 5.95um. It shows that the non-polar GaN thin film prepared by the utility model has very good performance in optical properties.

图4为本实施例制备的生长在LiGaO2衬底上的非极性m面蓝光LED外延片的在温度为室温下EL谱测试图。由图可知,温度为293K下EL谱测试得到发光峰波长为450nm,半峰宽为22nm,输出功率为1.5mw20mA,光照度为0.05lm。表明本实用新型制备的非极性GaN薄膜在电学性质上具有非常好的性能。Fig. 4 is an EL spectrum test chart of the non-polar m-plane blue LED epitaxial wafer grown on the LiGaO 2 substrate prepared in this embodiment at room temperature. It can be seen from the figure that the EL spectrum test at the temperature of 293K results in a luminous peak wavelength of 450nm, a half-maximum width of 22nm, an output power of 1.5mw20mA, and an illuminance of 0.05lm. It shows that the non-polar GaN film prepared by the utility model has very good performance in electrical properties.

实施例2Example 2

本实施例生长在LiGaO2衬底上的非极性蓝光LED外延片的制备方法,包括以下步骤:The preparation method of the non-polar blue light LED epitaxial wafer grown on the LiGaO2 substrate in this embodiment comprises the following steps:

(1)采用LiGaO2衬底,选取晶体取向为(100)晶面偏向(110)方向0.5°;(1) Using LiGaO 2 substrate, the crystal orientation is selected as (100) crystal plane biased to (110) direction by 0.5°;

(2)对衬底进行退火处理:将衬底在1000℃下高温烘烤5h后空冷至室温;(2) Annealing the substrate: bake the substrate at 1000°C for 5 hours, then air cool to room temperature;

(3)对衬底进行表面清洁处理:将LiGaO2衬底放入去离子水中室温下超声清洗10分钟,去除LiGaO2衬底表面粘污颗粒,再依次经过盐酸、丙酮、乙醇洗涤,去除表面有机物;清洗后的LiGaO2衬底用高纯干燥氮气吹干;之后将LiGaO2衬底放入低温分子束外延生长室,在超高真空条件下,将衬底温度升至900℃,烘烤30分钟,除去LiGaO2衬底表面残余的杂质;(3) Surface cleaning of the substrate: Put the LiGaO 2 substrate into deionized water and ultrasonically clean it at room temperature for 10 minutes to remove the sticky dirt particles on the surface of the LiGaO 2 substrate, and then wash with hydrochloric acid, acetone, and ethanol in sequence to remove the surface Organic matter; the cleaned LiGaO 2 substrate is dried with high-purity dry nitrogen; then the LiGaO 2 substrate is placed in a low-temperature molecular beam epitaxy growth chamber, and the substrate temperature is raised to 900°C under ultra-high vacuum conditions, and baked 30 minutes, remove LiGaO 2 residual impurities on the substrate surface;

(4)采用低温分子束外延工艺生长非极性m面GaN缓冲层,工艺条件为:衬底温度为350℃,通入Ga蒸发源与N等离子体,反应室压力为7×10-5torr、产生等离子体氮的射频功率为300W,Ⅴ/Ⅲ比为60、生长速度为0.6ML/s;(4) The non-polar m-plane GaN buffer layer is grown by low-temperature molecular beam epitaxy. The process conditions are: the substrate temperature is 350°C, the Ga evaporation source and N plasma are introduced, and the reaction chamber pressure is 7×10 -5 torr , The radio frequency power for generating plasma nitrogen is 300W, the V/III ratio is 60, and the growth rate is 0.6ML/s;

(5)采用脉冲激光沉积工艺生长非极性m面GaN外延层,工艺条件为:衬底温度升至550℃,采用脉冲激光轰击Ga靶材,同时通入N2,反应室压力为5×10-5torr,激光能量为180mJ,激光频率为30Hz;(5) The non-polar m-plane GaN epitaxial layer was grown by pulsed laser deposition process. The process conditions were as follows: the substrate temperature was raised to 550°C, the pulsed laser was used to bombard the Ga target, and N 2 was introduced at the same time, and the pressure of the reaction chamber was 5× 10 -5 torr, laser energy 180mJ, laser frequency 30Hz;

(6)采用分子束外延工艺生长非极性非掺杂u-GaN层,工艺条件为:衬底温度为800℃,通入Ga蒸发源与N等离子体,反应室压力为7×10-5torr、产生等离子体氮的射频功率为300W;(6) The non-polar and non-doped u-GaN layer is grown by molecular beam epitaxy. The process conditions are: the substrate temperature is 800°C, the Ga evaporation source and N plasma are introduced, and the reaction chamber pressure is 7×10 -5 torr, the RF power for generating plasma nitrogen is 300W;

(7)采用脉冲激光沉积工艺生长非极性n型掺杂GaN薄膜,工艺条件为:衬底温度为550℃,采用脉冲激光轰击GaSi混合靶材,生长时通入N等离子体,反应室压力为7×10-5torr、射频功率为300W,激光能量为180mJ,激光频率为30Hz,掺杂电子浓度5.0×1019cm-3(7) The non-polar n-type doped GaN film is grown by pulsed laser deposition process. The process conditions are as follows: the substrate temperature is 550°C, the pulsed laser is used to bombard the GaSi mixed target, N plasma is introduced during the growth, and the pressure of the reaction chamber is 7×10 -5 torr, RF power 300W, laser energy 180mJ, laser frequency 30Hz, doped electron concentration 5.0×10 19 cm -3 ;

(8)采用分子束外延工艺生长非极性InGaN/GaN量子阱,工艺条件为:衬底温度为750℃,通入Ga蒸发源与N等离子体,反应室压力为7×10-5torr,产生等离子体氮的射频功率为300W;(8) Non-polar InGaN/GaN quantum wells are grown by molecular beam epitaxy. The process conditions are as follows: substrate temperature is 750°C, Ga evaporation source and N plasma are introduced, and reaction chamber pressure is 7×10 -5 torr. The RF power for generating plasma nitrogen is 300W;

(9)采用脉冲激光沉积工艺生长非极性p型掺杂GaN薄膜,工艺条件为:衬底温度为550℃,采用脉冲激光轰击GaMg混合靶材来生长p型GaN薄膜,生长时通入N等离子体,反应室压力为7×10-5torr,射频功率为300W,激光能量为180mJ,激光频率为30Hz,空穴载流子浓度由GaMg混合靶材中两种元素的原子比来控制,掺杂空穴浓度2.0×1018cm-3(9) The non-polar p-type doped GaN film is grown by pulsed laser deposition process. The process conditions are as follows: the substrate temperature is 550°C, the pulsed laser is used to bombard the GaMg mixed target to grow the p-type GaN film, and the N Plasma, the reaction chamber pressure is 7×10 -5 torr, the radio frequency power is 300W, the laser energy is 180mJ, the laser frequency is 30Hz, the hole carrier concentration is controlled by the atomic ratio of the two elements in the GaMg mixed target, The doping hole concentration is 2.0×10 18 cm -3 .

本实施例制备的生长在LiGaO2衬底上的非极性蓝光LED外延片,包括由下至上依次排列的LiGaO2衬底、非极性m面GaN缓冲层、非极性m面GaN外延层、非极性非掺杂u-GaN层、非极性n型掺杂GaN薄膜、非极性InGaN/GaN量子阱层、非极性p型掺杂GaN薄膜;其中,所述非极性m面GaN缓冲层的厚度为60nm;所述非极性m面GaN外延层的厚度为250nm;非极性非掺杂u-GaN层的厚度为500nm;所述非极性n型掺杂GaN层的厚度为5μm;所述非极性InGaN/GaN量子阱层为10个周期的InGaN阱层/GaN垒层,其中InGaN阱层的厚度为3nm;GaN垒层的厚度为13nm;所述非极性p型掺杂GaN薄膜的厚度为500nm。The nonpolar blue LED epitaxial wafer grown on the LiGaO 2 substrate prepared in this example includes a LiGaO 2 substrate, a nonpolar m-plane GaN buffer layer, and a nonpolar m-plane GaN epitaxial layer arranged in sequence from bottom to top. , non-polar non-doped u-GaN layer, non-polar n-type doped GaN film, non-polar InGaN/GaN quantum well layer, non-polar p-type doped GaN film; wherein, the non-polar m The thickness of the GaN buffer layer is 60nm; the thickness of the non-polar m-plane GaN epitaxial layer is 250nm; the thickness of the non-polar non-doped u-GaN layer is 500nm; the non-polar n-type doped GaN layer The thickness of the InGaN/GaN quantum well layer is 10 cycles of InGaN well layer/GaN barrier layer, wherein the thickness of the InGaN well layer is 3nm; the thickness of the GaN barrier layer is 13nm; the nonpolar The thickness of the p-type doped GaN thin film is 500nm.

上述实施例为本实用新型较佳的实施方式,但本实用新型的实施方式并不受所述实施例的限制,其他的任何未背离本实用新型的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本实用新型的保护范围之内。The above-mentioned embodiment is a preferred implementation mode of the present utility model, but the implementation mode of the present utility model is not limited by the described embodiment, and any other changes, modifications, modifications, Substitution, combination, and simplification should all be equivalent replacement methods, and are all included in the protection scope of the present utility model.

Claims (3)

1.生长在LiGaO2衬底上的非极性蓝光LED外延片,其特征在于,包括由下至上依次排列的LiGaO2衬底、非极性m面GaN缓冲层、非极性m面GaN外延层、非极性非掺杂u-GaN层、非极性n型掺杂GaN薄膜、非极性InGaN/GaN量子阱层、非极性p型掺杂GaN薄膜。1. A nonpolar blue LED epitaxial wafer grown on a LiGaO2 substrate, characterized in that it comprises a LiGaO2 substrate, a nonpolar m-plane GaN buffer layer, and a nonpolar m-plane GaN epitaxial wafer arranged in sequence from bottom to top. Layer, non-polar non-doped u-GaN layer, non-polar n-type doped GaN film, non-polar InGaN/GaN quantum well layer, non-polar p-type doped GaN film. 2.根据权利要求1所述的生长在LiGaO2衬底上的非极性蓝光LED外延片,其特征在于,所述LiGaO2衬底的晶体取向为(100)晶面偏向(110)方向0.2~0.5°。2. The non-polar blue LED epitaxial wafer grown on LiGaO2 substrate according to claim 1, characterized in that, the crystal orientation of said LiGaO2 substrate is (100) crystal plane biased to (110) direction 0.2 ~0.5°. 3.根据权利要求1所述的生长在LiGaO2衬底上的非极性蓝光LED外延片,其特征在于,所述非极性m面GaN缓冲层的厚度为30~60nm;所述非极性m面GaN外延层的厚度为150~250nm;非极性非掺杂GaN层的厚度为300~500nm;所述非极性n型掺杂GaN层的厚度为3~5μm;所述非极性InGaN/GaN量子阱层为5~10个周期的InGaN阱层/GaN垒层,其中InGaN阱层的厚度为2~3nm;GaN垒层的厚度为10~13nm;所述非极性p型掺杂GaN薄膜的厚度为350~500nm,所述非极性n型掺杂GaN薄膜的电子浓度为1.0×1017~5.0×1019cm-3;所述非极性p型掺杂GaN薄膜的空穴浓度为1.0×1016~2.0×1018cm-33. the nonpolar blue light LED epitaxial wafer grown on LiGaO2 substrate according to claim 1, is characterized in that, the thickness of described nonpolar m-plane GaN buffer layer is 30~60nm; The thickness of the polar m-plane GaN epitaxial layer is 150-250 nm; the thickness of the non-polar non-doped GaN layer is 300-500 nm; the thickness of the non-polar n-type doped GaN layer is 3-5 μm; the non-polar The permanent InGaN/GaN quantum well layer is an InGaN well layer/GaN barrier layer with 5~10 cycles, wherein the thickness of the InGaN well layer is 2~3nm; the thickness of the GaN barrier layer is 10~13nm; the nonpolar p-type The thickness of the doped GaN film is 350-500 nm, the electron concentration of the non-polar n-type doped GaN film is 1.0×10 17 ~5.0×10 19 cm -3 ; the non-polar p-type doped GaN film The hole concentration is 1.0×10 16 ~2.0×10 18 cm -3 .
CN 201220684170 2012-12-11 2012-12-11 Non-polar blue LED epitaxial wafer grown on LiGaO2 substrate Expired - Lifetime CN203085627U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103035789A (en) * 2012-12-11 2013-04-10 华南理工大学 Non-polar blue LED epitaxial wafer grown on LiGaO2 substrate and preparation method thereof
CN103996758A (en) * 2014-05-30 2014-08-20 广州市众拓光电科技有限公司 LED epitaxial wafer growing on Cu substrate and preparing method and application of LED epitaxial wafer
RU2643176C1 (en) * 2014-03-24 2018-01-31 Шанхай Чиптек Сэмикондактор Текнолоджи Ко., Лтд. Non-polar led epitaxial plate of blue glow on substrate of lao and method of its production
WO2018076407A1 (en) * 2016-10-31 2018-05-03 华南理工大学 Nonpolar nanorod led grown on lithium gallate substrate and preparation method therefor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103035789A (en) * 2012-12-11 2013-04-10 华南理工大学 Non-polar blue LED epitaxial wafer grown on LiGaO2 substrate and preparation method thereof
CN103035789B (en) * 2012-12-11 2015-08-26 华南理工大学 Growth is at LiGaO 2nonpolar blue-ray LED epitaxial wafer on substrate and preparation method thereof
RU2643176C1 (en) * 2014-03-24 2018-01-31 Шанхай Чиптек Сэмикондактор Текнолоджи Ко., Лтд. Non-polar led epitaxial plate of blue glow on substrate of lao and method of its production
CN103996758A (en) * 2014-05-30 2014-08-20 广州市众拓光电科技有限公司 LED epitaxial wafer growing on Cu substrate and preparing method and application of LED epitaxial wafer
WO2018076407A1 (en) * 2016-10-31 2018-05-03 华南理工大学 Nonpolar nanorod led grown on lithium gallate substrate and preparation method therefor

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