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CN102637787B - Method for uninterrupted growth of high-quality InGaN/GaN multi-quantum well (MQW) - Google Patents

Method for uninterrupted growth of high-quality InGaN/GaN multi-quantum well (MQW) Download PDF

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CN102637787B
CN102637787B CN201210124792.4A CN201210124792A CN102637787B CN 102637787 B CN102637787 B CN 102637787B CN 201210124792 A CN201210124792 A CN 201210124792A CN 102637787 B CN102637787 B CN 102637787B
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李盼盼
李鸿渐
张逸韵
李志聪
梁萌
李璟
王国宏
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Abstract

本发明公开了一种无间断生长高质量InGaN/GaN多量子阱的方法,包括:在蓝宝石图形衬底上外延生长uGaN,在uGaN上生长nGaN,然后在nGaN上生长MQW应力释放层;在MQW应力释放层上外延生长InGaN/GaN多量子阱;在InGaN/GaN多量子阱上重复生长多个InGaN/GaN多量子阱;在该多个InGaN/GaN多量子阱上生长GaN基LED所需的pAlGaN和pGaN。本发明选用金属有机物化学气相沉积法,利用在切换量子阱和垒生长条件过程中保持GaN生长,即进行量子阱无间断生长,缩短了多量子阱生长所需的时间,大大提高了生产效率,同时获取高质量InGaN/GaN多量子阱的LED外延片。

The invention discloses a method for growing high-quality InGaN/GaN multiple quantum wells without interruption, comprising: epitaxially growing uGaN on a sapphire pattern substrate, growing nGaN on the uGaN, and then growing an MQW stress release layer on the nGaN; Epitaxial growth of InGaN/GaN multiple quantum wells on the stress release layer; repeated growth of multiple InGaN/GaN multiple quantum wells on the InGaN/GaN multiple quantum wells; growth of GaN-based LEDs on the multiple InGaN/GaN multiple quantum wells pAlGaN and pGaN. The present invention selects the metal-organic chemical vapor deposition method, utilizes the growth of GaN during the process of switching quantum wells and barrier growth conditions, that is, performs quantum well growth without interruption, shortens the time required for multi-quantum well growth, and greatly improves production efficiency. At the same time, high-quality InGaN/GaN multi-quantum well LED epitaxial wafers are obtained.

Description

一种无间断生长高质量InGaN/GaN多量子阱的方法A Method for Uninterrupted Growth of High Quality InGaN/GaN Multiple Quantum Wells

技术领域 technical field

本发明涉及量子阱生长技术领域,特别是一种无间断生长高质量InGaN/GaN多量子阱的方法,适用于高亮度GaN基LED外延片商业化生产。The invention relates to the technical field of quantum well growth, in particular to a method for growing high-quality InGaN/GaN multiple quantum wells without interruption, which is suitable for commercial production of high-brightness GaN-based LED epitaxial wafers.

背景技术 Background technique

GaN基LED目前已经进入商业化生产阶段,如何缩短GaN基LED外延片生长时间同时获得高质量外延片以提高产能成为了一个研究重点。目前均采用MOCVD进行GaN基LED外延片商业化生产。由于InGaN量子阱和GaN量子垒生长温度气氛存在差别,在生长InGaN/GaN多量子阱过程中有很多时间用于切换量子阱和量子垒生长所需的温度和气氛,切换过程中为了保证外延材料质量一般不进行外延生长,因此在生长量子阱过程中存在间断生长,时间利用率不高。目前在MOCVD外延生长GaN基LED制作工艺中,MQWs生长时间占据了GaN基LED外延片生长所需的一半时间,如何缩短MQWs生长时间成为提高GaN基LED外延片生产效率的一个主要因素。GaN-based LEDs have now entered the stage of commercial production. How to shorten the growth time of GaN-based LED epitaxial wafers while obtaining high-quality epitaxial wafers to increase production capacity has become a research focus. At present, MOCVD is used for commercial production of GaN-based LED epitaxial wafers. Due to the differences in the growth temperature and atmosphere between InGaN quantum wells and GaN quantum barriers, there is a lot of time spent in switching the temperature and atmosphere required for the growth of quantum wells and quantum barriers during the growth of InGaN/GaN multiple quantum wells. Quality generally does not undergo epitaxial growth, so there is intermittent growth during the growth of quantum wells, and the time utilization rate is not high. At present, in the MOCVD epitaxial growth GaN-based LED manufacturing process, the growth time of MQWs occupies half of the time required for the growth of GaN-based LED epitaxial wafers. How to shorten the MQWs growth time has become a major factor in improving the production efficiency of GaN-based LED epitaxial wafers.

发明内容 Contents of the invention

(一)要解决的技术问题(1) Technical problems to be solved

有鉴于此,本发明的主要目的在于提供一种无间断生长高质量InGaN/GaN多量子阱的方法,以缩短多量子阱生长所需的时间,提高生产效率,获取高质量InGaN/GaN多量子阱的LED外延片。In view of this, the main purpose of the present invention is to provide a method for growing high-quality InGaN/GaN multiple quantum wells without interruption, to shorten the time required for the growth of multiple quantum wells, improve production efficiency, and obtain high-quality InGaN/GaN multiple quantum wells well for the LED epiwafer.

(二)技术方案(2) Technical solution

为达到上述目的,本发明提供了一种无间断生长高质量InGaN/GaN多量子阱的方法,该方法包括:In order to achieve the above object, the present invention provides a method for growing high-quality InGaN/GaN multiple quantum wells without interruption, the method comprising:

在蓝宝石图形衬底上外延生长uGaN1,接着在uGaN1上生长nGaN2,然后在nGaN2上生长MQW应力释放层3;Epitaxially grow uGaN1 on the sapphire pattern substrate, then grow nGaN2 on uGaN1, and then grow MQW stress release layer 3 on nGaN2;

在MQW应力释放层3上外延生长InGaN/GaN多量子阱;Epitaxial growth of InGaN/GaN multiple quantum wells on the MQW stress release layer 3;

在InGaN/GaN多量子阱上重复生长多个InGaN/GaN多量子阱;Repeated growth of multiple InGaN/GaN multiple quantum wells on InGaN/GaN multiple quantum wells;

在该多个InGaN/GaN多量子阱上生长GaN基LED所需的pA1GaN12和pGaN13。The pAlGaN12 and pGaN13 required for GaN-based LEDs are grown on the multiple InGaN/GaN multiple quantum wells.

上述方案中,所述MQW应力释放层3采用的是InGaN与GaN的超晶格结构,包括m个铟镓氮(InyGa1-yN)量子阱与m+1个氮化镓(GaN)量子势垒,每个InyGa1-yN量子阱上下两侧都有一个GaN量子垒,其中m≥1,0≤y≤1;GaN的厚度在之间,InGaN的厚度在之间。In the above scheme, the MQW stress release layer 3 adopts a superlattice structure of InGaN and GaN, including m indium gallium nitride (In y Ga 1-y N) quantum wells and m+1 gallium nitride (GaN ) quantum barrier, each In y Ga 1-y N quantum well has a GaN quantum barrier on the upper and lower sides, where m≥1, 0≤y≤1; the thickness of GaN is in arrive Between, the thickness of InGaN is in arrive between.

上述方案中,该InGaN/GaN多量子阱由下至上依次包括InGaN量子阱4、第一GaN覆盖层5、升温层6、第一稳温层7、量子垒(QB)8、降温层9、第二稳温层10和第二GaN覆盖层11。所述在MQW应力释放层3上外延生长InGaN/GaN多量子阱,包括:在MQW应力释放层3上外延生长InGaN量子阱4;在InGaN量子阱4上生长第一GaN覆盖层5;在第一GaN覆盖层5上生长升温层6;在升温层6上生长第一稳温层7;在第一稳温层7上生长GaN量子垒8;在GaN量子垒8上生长降温层9;在降温层9上生长第二稳温层10;以及在第二稳温层10上生长第二GaN覆盖层11,形成一InGaN/GaN多量子阱。In the above scheme, the InGaN/GaN multiple quantum wells sequentially include an InGaN quantum well 4, a first GaN cladding layer 5, a heating layer 6, a first temperature stabilizing layer 7, a quantum barrier (QB) 8, a cooling layer 9, The second temperature stabilizing layer 10 and the second GaN capping layer 11 . The epitaxial growth of InGaN/GaN multiple quantum wells on the MQW stress release layer 3 includes: epitaxially growing InGaN quantum wells 4 on the MQW stress release layer 3; growing a first GaN cladding layer 5 on the InGaN quantum wells 4; A temperature rising layer 6 is grown on the GaN cladding layer 5; a first temperature stabilizing layer 7 is grown on the temperature rising layer 6; a GaN quantum barrier 8 is grown on the first temperature stabilizing layer 7; a cooling layer 9 is grown on the GaN quantum barrier 8; growing a second temperature stabilizing layer 10 on the cooling layer 9; and growing a second GaN capping layer 11 on the second temperature stabilizing layer 10 to form an InGaN/GaN multiple quantum well.

上述方案中,所述在MQW应力释放层3上外延生长InGaN量子阱4,选用高纯N2做载气,厚度在之间,量子阱生长温度(QW_T)在750℃~900℃之间,In组分在0%~50%之间,选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。In the above scheme, the InGaN quantum well 4 is epitaxially grown on the MQW stress release layer 3, and high -purity N is used as the carrier gas, with a thickness of Between, the quantum well growth temperature (QW_T) is between 750°C and 900°C, the In composition is between 0% and 50%, and SiH 4 is selected for n-type doping, and the doping concentration is between 1.0E+17cm - Between 3 and 5.0E+19cm -3 .

上述方案中,所述在InGaN量子阱4上生长第一GaN覆盖层5,选用高纯N2做载气,厚度在之间,生长温度与QW_T相同,可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。In the above scheme, the first GaN cladding layer 5 is grown on the InGaN quantum well 4, and high -purity N is used as the carrier gas, with a thickness of Between, the growth temperature is the same as that of QW_T, SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

上述方案中,所述在第一GaN覆盖层5上生长升温层6,选用GaN材料,同时通入高纯N2和高纯H2混合气做载气,N2和H2比例:1=<N2/H2<=100,三乙基镓(TEGa)作为镓源,厚度在之间,生长过程中温度始终处于变化的状态,温度从开始的QW_T一直上升到量子垒生长温度(QB_T),QB_T在800℃~1000℃之间,比QB_T高40℃以上。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。In the above-mentioned scheme, the temperature raising layer 6 is grown on the first GaN cladding layer 5, GaN material is selected, and high-purity N2 and high-purity H2 mixed gas is introduced at the same time as the carrier gas, and the ratio of N2 and H2 is: 1= <N 2 /H 2 <=100, triethylgallium (TEGa) is used as gallium source, the thickness is During the growth process, the temperature is always in a state of change. The temperature rises from the initial QW_T to the quantum barrier growth temperature (QB_T). QB_T is between 800°C and 1000°C, which is more than 40°C higher than QB_T. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

上述方案中,所述在升温层6上生长第一稳温层7,选用GaN材料,高纯N2和高纯H2混合气体做载气,N2和H2比例:1=<N2/H2<=100,生长过程中设定温度始终保持在QB_T,时间持续在10s~600s。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。In the above scheme, the first temperature stabilizing layer 7 is grown on the temperature raising layer 6, GaN material is selected, and the mixed gas of high-purity N2 and high-purity H2 is used as the carrier gas, and the ratio of N2 and H2 is: 1=< N2 /H 2 <=100, the set temperature is always kept at QB_T during the growth process, and the time lasts for 10s~600s. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

上述方案中,所述在第一稳温层7上生长GaN量子垒8,选择GaN材料,同时通入高纯N2和高纯H2混合气做载气,N2和H2比例:1=<N2/H2<=100,厚度在之间,生长温度保持在QB_T。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。In the above scheme, the GaN quantum barrier 8 is grown on the first temperature stabilizing layer 7, the GaN material is selected, and high-purity N2 and high-purity H2 mixed gas is introduced as the carrier gas at the same time, and the ratio of N2 and H2 is: 1 =<N 2 /H 2 <=100, the thickness is arrive Between, the growth temperature is kept at QB_T. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

上述方案中,所述在GaN量子垒8上生长降温层9,选择GaN材料,同时通入高纯N2和高纯H2混合气体做载气,N2和H2比例:1=<N2/H2<=100,厚度在之间,生长温度从QB_T下降到QW_T。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。In the above scheme, the cooling layer 9 is grown on the GaN quantum barrier 8, the GaN material is selected, and the mixed gas of high-purity N2 and high-purity H2 is introduced at the same time as the carrier gas, and the ratio of N2 and H2 is: 1=<N 2 /H 2 <=100, the thickness is arrive Between, the growth temperature drops from QB_T to QW_T. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

上述方案中,所述在降温层9上生长第二稳温层10,选用GaN材料,同时通入高纯N2和高纯H2混合气体做载气,N2和H2比例:1=<N2/H2<=100,厚度在之间,生长温度保持在QW_T,时间持续在10s~600s。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。In the above scheme, the second temperature stabilizing layer 10 is grown on the cooling layer 9, GaN material is selected, and high-purity N2 and high-purity H2 mixed gas is introduced as the carrier gas at the same time, and the ratio of N2 and H2 is: 1= <N 2 /H 2 <=100, the thickness is arrive Between, the growth temperature is kept at QW_T, and the time lasts from 10s to 600s. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

上述方案中,所述在第二稳温层10上生长第二GaN覆盖层11,采用高纯N2做载气,厚度在之间,生长温度与QW_T相同。In the above scheme, the second GaN capping layer 11 is grown on the second temperature stabilizing layer 10, and high-purity N2 is used as the carrier gas, with a thickness of Between, the growth temperature is the same as QW_T.

上述方案中,所述在InGaN/GaN多量子阱上重复生长多个InGaN/GaN多量子阱,InGaN/GaN多量子阱的个数为N,且1=<N<=25。In the above solution, multiple InGaN/GaN multiple quantum wells are repeatedly grown on the InGaN/GaN multiple quantum wells, the number of InGaN/GaN multiple quantum wells is N, and 1=<N<=25.

(三)有益效果(3) Beneficial effects

从上述技术方案可以看出,本发明具有以下有益效果:As can be seen from the foregoing technical solutions, the present invention has the following beneficial effects:

本发明提供的这种无间断生长高质量InGaN/GaN多量子阱的方法,选用金属有机物化学气相沉积(MOCVD)法,利用在切换量子阱和垒生长条件过程中保持GaN生长,即进行量子阱无间断生长,缩短了多量子阱生长所需的时间,大大提高了生产效率,同时获取高质量InGaN/GaN多量子阱的LED外延片。The method for growing high-quality InGaN/GaN multi-quantum wells without interruption provided by the present invention adopts the metal organic chemical vapor deposition (MOCVD) method, and utilizes the method of maintaining GaN growth in the process of switching quantum wells and barrier growth conditions, that is, performing quantum well The uninterrupted growth shortens the time required for the growth of multiple quantum wells, greatly improves the production efficiency, and at the same time obtains high-quality InGaN/GaN multi-quantum well LED epitaxial wafers.

附图说明 Description of drawings

图1是依照本发明实施例的无间断生长高质量InGaN/GaN多量子阱的方法流程图;1 is a flowchart of a method for growing high-quality InGaN/GaN multiple quantum wells without interruption according to an embodiment of the present invention;

图2是依照本发明实施例的采用无间断生长InGaN/GaN多量子阱LED外延结构的示意图;2 is a schematic diagram of an epitaxial structure of an InGaN/GaN multi-quantum well LED grown without interruption according to an embodiment of the present invention;

图3是依照本发明实施例采用本发明获得的GaN基蓝光LED外延片的PL谱;Fig. 3 is the PL spectrum of the GaN-based blue LED epitaxial wafer obtained by the present invention according to an embodiment of the present invention;

图4是依照本发明实施例采用本发明获得的GaN基蓝光LED外延片(002)方向ω-2θXRD衍射谱。Fig. 4 is an ω-2θ XRD diffraction spectrum of a GaN-based blue LED epitaxial wafer (002) direction obtained by using the present invention according to an embodiment of the present invention.

具体实施方式 Detailed ways

为使本发明的目的、技术方案和优点更加清楚明白,以下结合具体实施例,并参照附图,对本发明进一步详细说明。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be described in further detail below in conjunction with specific embodiments and with reference to the accompanying drawings.

如图1所示,图1是依照本发明实施例的无间断生长高质量InGaN/GaN多量子阱的方法流程图,该方法包括:As shown in FIG. 1, FIG. 1 is a flow chart of a method for growing high-quality InGaN/GaN multiple quantum wells without interruption according to an embodiment of the present invention. The method includes:

步骤1:在蓝宝石图形衬底上外延生长未掺杂氮化镓(uGaN)1,接着在uGaN1上生长n型氮化镓(nGaN)2,然后在nGaN2上生长InGaN/GaN多量子阱(MQW)应力释放层3;Step 1: Epitaxially grow undoped gallium nitride (uGaN)1 on a sapphire pattern substrate, then grow n-type gallium nitride (nGaN)2 on uGaN1, and then grow InGaN/GaN multiple quantum wells (MQW) on nGaN2 ) stress release layer 3;

步骤2:在MQW应力释放层3上外延生长InGaN/GaN多量子阱;Step 2: epitaxially grow InGaN/GaN multiple quantum wells on the MQW stress release layer 3;

步骤3:在InGaN/GaN多量子阱上重复生长多个InGaN/GaN多量子阱;Step 3: repeatedly growing multiple InGaN/GaN multiple quantum wells on the InGaN/GaN multiple quantum wells;

步骤4:在该多个InGaN/GaN多量子阱上生长GaN基LED所需的p型铝镓氮(pAlGaN)12和p型氮化镓(pGaN)13。Step 4: growing p-type aluminum gallium nitride (pAlGaN) 12 and p-type gallium nitride (pGaN) 13 required for GaN-based LEDs on the multiple InGaN/GaN multiple quantum wells.

步骤1中所述MQW应力释放层3采用的是InGaN与GaN的超晶格结构,包括m个铟镓氮(InyGa1-yN)量子阱与m+1个氮化镓(GaN)量子势垒,每个InyGa1-yN量子阱上下两侧都有一个GaN量子垒,其中m≥1,0≤y≤1;GaN的厚度在之间,InGaN的厚度在之间。The MQW stress release layer 3 described in step 1 adopts a superlattice structure of InGaN and GaN, including m indium gallium nitride (In y Ga 1-y N) quantum wells and m+1 gallium nitride (GaN) Quantum barriers, each In y Ga 1-y N quantum well has a GaN quantum barrier on the upper and lower sides, where m≥1, 0≤y≤1; the thickness of GaN is arrive Between, the thickness of InGaN is in arrive between.

步骤2中所述InGaN/GaN多量子阱由下至上依次包括InGaN量子阱4、第一GaN覆盖层5、升温层6、第一稳温层7、量子垒(QB)8、降温层9、第二稳温层10和第二GaN覆盖层11。所述在MQW应力释放层3上外延生长InGaN/GaN多量子阱,包括:在MQW应力释放层3上外延生长InGaN量子阱4;在InGaN量子阱4上生长第一GaN覆盖层5;在第一GaN覆盖层5上生长升温层6;在升温层6上生长第一稳温层7;在第一稳温层7上生长GaN量子垒8;在GaN量子垒8上生长降温层9;在降温层9上生长第二稳温层10;以及在第二稳温层10上生长第二GaN覆盖层11,形成一InGaN/GaN多量子阱。The InGaN/GaN multi-quantum well described in step 2 includes, from bottom to top, an InGaN quantum well 4, a first GaN cladding layer 5, a heating layer 6, a first temperature stabilizing layer 7, a quantum barrier (QB) 8, a cooling layer 9, The second temperature stabilizing layer 10 and the second GaN capping layer 11 . The epitaxial growth of InGaN/GaN multiple quantum wells on the MQW stress release layer 3 includes: epitaxially growing InGaN quantum wells 4 on the MQW stress release layer 3; growing a first GaN cladding layer 5 on the InGaN quantum wells 4; A temperature rising layer 6 is grown on the GaN cladding layer 5; a first temperature stabilizing layer 7 is grown on the temperature rising layer 6; a GaN quantum barrier 8 is grown on the first temperature stabilizing layer 7; a cooling layer 9 is grown on the GaN quantum barrier 8; growing a second temperature stabilizing layer 10 on the cooling layer 9; and growing a second GaN capping layer 11 on the second temperature stabilizing layer 10 to form an InGaN/GaN multiple quantum well.

其中,所述在MQW应力释放层3上外延生长InGaN量子阱4,选用高纯N2做载气,厚度在之间,量子阱生长温度(QW_T)在750℃~900℃之间,In组分在0%~50%之间,选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。Wherein, the InGaN quantum well 4 is epitaxially grown on the MQW stress release layer 3, and high -purity N is selected as the carrier gas, and the thickness is between Between, the quantum well growth temperature (QW_T) is between 750°C and 900°C, the In composition is between 0% and 50%, and SiH 4 is selected for n-type doping, and the doping concentration is between 1.0E+17cm - Between 3 and 5.0E+19cm -3 .

所述在InGaN量子阱4上生长第一GaN覆盖层5,选用高纯N2做载气,厚度在之间,生长温度与QW_T相同,可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。The first GaN capping layer 5 is grown on the InGaN quantum well 4, and high -purity N is used as the carrier gas, with a thickness of Between, the growth temperature is the same as that of QW_T, SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

所述在第一GaN覆盖层5上生长升温层6,选用GaN材料,同时通入高纯N2和高纯H2混合气做载气,N2和H2比例:1=<N2/H2<=100,三乙基镓(TEGa)作为镓源,厚度在之间,生长过程中温度始终处于变化的状态,温度从开始的QW_T一直上升到量子垒生长温度(QB_T),QB_T在800℃~1000℃之间,比QB_T高40℃以上。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。The temperature raising layer 6 is grown on the first GaN capping layer 5, GaN material is selected, and high-purity N 2 and high-purity H 2 mixed gas is introduced as the carrier gas at the same time, and the ratio of N 2 and H 2 is: 1=<N 2 / H 2 <=100, triethylgallium (TEGa) as gallium source, thickness in During the growth process, the temperature is always in a state of change. The temperature rises from the initial QW_T to the quantum barrier growth temperature (QB_T). QB_T is between 800°C and 1000°C, which is more than 40°C higher than QB_T. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

所述在升温层6上生长第一稳温层7,选用GaN材料,高纯N2和高纯H2混合气体做载气,N2和H2比例:1=<N2/H2<=100,生长过程中设定温度始终保持在QB_T,时间持续在10s~600s。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。The first temperature stabilizing layer 7 is grown on the temperature raising layer 6, using GaN material, high-purity N 2 and high-purity H 2 mixed gas as carrier gas, the ratio of N 2 and H 2 : 1=<N 2 /H 2 < =100, the set temperature is always kept at QB_T during the growth process, and the time lasts from 10s to 600s. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

所述在第一稳温层7上生长GaN量子垒8,选择GaN材料,同时通入高纯N2和高纯H2混合气做载气,N2和H2比例:1=<N2/H2<=100,厚度在之间,生长温度保持在QB_T。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。The GaN quantum barrier 8 is grown on the first temperature stabilization layer 7, GaN material is selected, and high-purity N 2 and high-purity H 2 mixed gas is introduced as the carrier gas at the same time, and the ratio of N 2 and H 2 is: 1=<N 2 /H 2 <=100, the thickness is arrive Between, the growth temperature is kept at QB_T. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

所述在GaN量子垒8上生长降温层9,选择GaN材料,同时通入高纯N2和高纯H2混合气体做载气,N2和H2比例:1=<N2/H2<=100,厚度在之间,生长温度从QB_T下降到QW_T。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。The cooling layer 9 is grown on the GaN quantum barrier 8, the GaN material is selected, and the mixed gas of high-purity N 2 and high-purity H 2 is introduced as the carrier gas at the same time, and the ratio of N 2 and H 2 is: 1=<N 2 /H 2 <=100, the thickness is arrive Between, the growth temperature drops from QB_T to QW_T. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

所述在降温层9上生长第二稳温层10,选用GaN材料,同时通入高纯N2和高纯H2混合气体做载气,N2和H2比例:1=<N2/H2<=100,厚度在之间,生长温度保持在QW_T,时间持续在10s~600s。可选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。The second temperature stabilizing layer 10 is grown on the cooling layer 9, GaN material is selected, and high-purity N 2 and high-purity H 2 mixed gas is introduced as the carrier gas at the same time, and the ratio of N 2 and H 2 is: 1=<N 2 / H 2 <=100, the thickness is arrive Between, the growth temperature is kept at QW_T, and the time lasts from 10s to 600s. SiH 4 can be used for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 .

所述在第二稳温层10上生长第二GaN覆盖层11,采用高纯N2做载气,厚度在之间,生长温度与QW_T相同。The second GaN capping layer 11 is grown on the second temperature stabilizing layer 10, using high -purity N as carrier gas, with a thickness of Between, the growth temperature is the same as QW_T.

步骤3中所述所述在InGaN/GaN多量子阱上重复生长多个InGaN/GaN多量子阱,InGaN/GaN多量子阱的个数为N,且1=<N<=25。In step 3, multiple InGaN/GaN multiple quantum wells are repeatedly grown on the InGaN/GaN multiple quantum wells, the number of InGaN/GaN multiple quantum wells is N, and 1=<N<=25.

实施例Example

利用MOCVD设备(Aixtron公司的Crius 31片商用机),选用高纯NH3作为N源,高纯N2和H2做载气,三甲基铟(TMIn)和三甲基铝(TMAl)分别作为铟源、铝源,三甲基镓(TMGa)作为GaN材料的镓源,三乙基镓(TEGa)作为InGaN/GaN多量子阱的镓源,硅烷(SiH4)为N型掺杂剂,二茂Mg(Cp2Mg)为P型掺杂剂。在蓝宝石图形衬底上外延生长uGaN1,接着在uGaN1上生长nGaN2,然后在nGaN2上生长MQW应力释放层3,该MQW应力释放层3采用的是InGaN/GaN的超晶格结构SLs,SLs对数为4,生长温度为900℃,在该InGaN/GaN的超晶格结构SLs中InGaN的厚度为GaN的厚度为 Utilize MOCVD equipment (Crius 31 commercial machines of Aixtron Company), select high-purity NH3 as N source, high-purity N2 and H2 as carrier gas, trimethylindium (TMIn) and trimethylaluminum (TMAl) respectively As the source of indium and aluminum, trimethylgallium (TMGa) as the source of gallium for GaN materials, triethylgallium (TEGa) as the source of gallium for InGaN/GaN multiple quantum wells, and silane (SiH 4 ) as the N-type dopant , Dioxocene Mg (Cp2Mg) is a P-type dopant. Epitaxially grow uGaN1 on the sapphire pattern substrate, then grow nGaN2 on uGaN1, and then grow MQW stress release layer 3 on nGaN2, the MQW stress release layer 3 adopts InGaN/GaN superlattice structure SLs, SLs logarithm is 4, the growth temperature is 900°C, and the thickness of InGaN in the InGaN/GaN superlattice structure SLs is The thickness of GaN is

选用高纯N2做载气,在MQW应力释放层3上外延生长InGaN量子阱4。生长温度为800℃,厚度为紧接着在InGaN量子阱4上生长第一GaN覆盖层5,温度同为800℃,厚度为然后在第一GaN覆盖层5上生长升温层6,生长温度从800℃上升到890℃,生长气氛选用N2和H2混合气体,N2/H2比例为8,同时进行Si掺杂,掺杂浓度为2E+17cm-3。接着在升温层6上生长第一稳温层7,时间持续60s,持续通入Si,n型掺杂浓度为2E+17cm-3。接着在第一稳温层7上生长GaN量子垒8,温度为890℃,生长厚度为n型掺杂浓度为4E+17cm-3。接着在GaN量子垒8上生长降温层9,温度从890℃下降到800℃。接着在降温层9上生长第二稳温层10,时间持续60s。接着在第二稳温层10上生长第二GaN覆盖层11,采用高纯N2作为载气,停止通入H2,生长厚度为最终形成一InGaN/GaN多量子阱,该InGaN/GaN多量子阱由下至上依次包括InGaN量子阱4、第一GaN覆盖层5、升温层6、第一稳温层7、量子垒(QB)8、降温层9、第二稳温层10和第二GaN覆盖层11。High-purity N 2 is selected as the carrier gas, and the InGaN quantum well 4 is epitaxially grown on the MQW stress release layer 3 . The growth temperature is 800°C, and the thickness is Next, the first GaN capping layer 5 is grown on the InGaN quantum well 4 at the same temperature of 800°C and the thickness is Then grow the temperature raising layer 6 on the first GaN capping layer 5, the growth temperature is increased from 800°C to 890°C, the growth atmosphere is a mixed gas of N2 and H2 , the ratio of N2 / H2 is 8, and Si doping is carried out at the same time. The doping concentration is 2E+17cm -3 . Next, the first temperature stabilizing layer 7 is grown on the temperature raising layer 6 for 60 seconds, and Si is continuously injected, and the n-type doping concentration is 2E+17cm −3 . Next, a GaN quantum barrier 8 is grown on the first temperature stabilizing layer 7 at a temperature of 890° C. and a growth thickness of The n-type doping concentration is 4E+17cm -3 . Next, a cooling layer 9 is grown on the GaN quantum barrier 8, and the temperature drops from 890°C to 800°C. Next, a second temperature stabilizing layer 10 is grown on the cooling layer 9 for 60 s. Next, the second GaN capping layer 11 is grown on the second temperature stabilizing layer 10, using high-purity N2 as the carrier gas, stopping the introduction of H2 , and the growth thickness is Finally, an InGaN/GaN multi-quantum well is formed, and the InGaN/GaN multi-quantum well includes an InGaN quantum well 4, a first GaN cladding layer 5, a heating layer 6, a first temperature stabilizing layer 7, and a quantum barrier (QB) from bottom to top. 8. A cooling layer 9 , a second temperature stabilizing layer 10 and a second GaN capping layer 11 .

重复以上步骤15次,即生长15个InGaN/GaN多量子阱。之后在该15个InGaN/GaN多量子阱上生长GaN基LED所需的pAlGaN12和pGaN13,具体如图2所示。Repeat the above steps 15 times, that is, grow 15 InGaN/GaN multiple quantum wells. Then pAlGaN12 and pGaN13 required for GaN-based LEDs are grown on the 15 InGaN/GaN multiple quantum wells, as shown in FIG. 2 .

获得的高质量GaN基LED PL谱如图3所示,可以看出半宽只有20nm。图4为所制备得到的高质量GaN基LED(002)方向XRD衍射谱,可以看出,InGaN/GaN多量子阱卫星峰明显,可以看到第五个卫星峰,说明采用本方法制备得到的InGaN/GaN多量子质量较好。The obtained high-quality GaN-based LED PL spectrum is shown in Figure 3, and it can be seen that the half width is only 20nm. Fig. 4 is the XRD diffraction spectrum of the prepared high-quality GaN-based LED (002) direction. It can be seen that the InGaN/GaN multi-quantum well satellite peak is obvious, and the fifth satellite peak can be seen, indicating that the method is used to prepare the obtained InGaN/GaN has better multi-quantum quality.

以上所述的具体实施例,对本发明的目的、技术方案和有益效果进行了进一步详细说明,所应理解的是,以上所述仅为本发明的具体实施例而已,并不用于限制本发明,凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The specific embodiments described above have further described the purpose, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above descriptions are only specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the protection scope of the present invention.

Claims (11)

1.一种无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,该方法包括:1. A method for growing high-quality InGaN/GaN multiple quantum wells without interruption, characterized in that the method comprises: 在蓝宝石图形衬底上外延生长uGaN(1),接着在uGaN(1)上生长nGaN(2),然后在nGaN(2)上生长MQW应力释放层(3);Epitaxial growth of uGaN (1) on a sapphire pattern substrate, followed by growth of nGaN (2) on uGaN (1), and then growth of an MQW stress release layer (3) on nGaN (2); 在MQW应力释放层(3)上外延生长InGaN/GaN多量子阱;Epitaxial growth of InGaN/GaN multiple quantum wells on the MQW stress release layer (3); 在InGaN/GaN多量子阱上重复生长多个InGaN/GaN多量子阱;Repeated growth of multiple InGaN/GaN multiple quantum wells on InGaN/GaN multiple quantum wells; 在该多个InGaN/GaN多量子阱上生长GaN基LED所需的pAlGaN(12)和pGaN(13);pAlGaN(12) and pGaN(13) required for growing GaN-based LEDs on the multiple InGaN/GaN multiple quantum wells; 其中,该InGaN/GaN多量子阱由下至上依次包括InGaN量子阱(4)、第一GaN覆盖层(5)、升温生长的GaN层(6)、第一稳温生长的GaN层(7)、量子垒(8)、降温生长的GaN层(9)、第二稳温生长的GaN层(10)和第二GaN覆盖层(11);所述在MQW应力释放层(3)上外延生长InGaN/GaN多量子阱,包括:Wherein, the InGaN/GaN multi-quantum well comprises, from bottom to top, an InGaN quantum well (4), a first GaN cladding layer (5), a GaN layer (6) grown at elevated temperature, and a first GaN layer (7) grown at a stable temperature. , a quantum barrier (8), a GaN layer (9) grown at reduced temperature, a second GaN layer (10) and a second GaN capping layer (11) grown at a stable temperature; the epitaxial growth on the MQW stress release layer (3) InGaN/GaN multiple quantum wells, including: 在MQW应力释放层(3)上外延生长InGaN量子阱(4);epitaxially growing InGaN quantum wells (4) on the MQW stress release layer (3); 在InGaN量子阱(4)上生长第一GaN覆盖层(5);growing a first GaN capping layer (5) on the InGaN quantum well (4); 在第一GaN覆盖层(5)上生长升温生长的GaN层(6);growing a temperature-increased GaN layer (6) on the first GaN capping layer (5); 在升温生长的GaN层(6)上生长第一稳温生长的GaN层(7);growing a first temperature-stable GaN layer (7) on the temperature-increased-grown GaN layer (6); 在第一稳温生长的GaN层(7)上生长GaN量子垒(8);growing a GaN quantum barrier (8) on the first stable temperature grown GaN layer (7); 在GaN量子垒(8)上生长降温生长的GaN层(9);growing a temperature-reduced GaN layer (9) on the GaN quantum barrier (8); 在降温生长的GaN层(9)上生长第二稳温生长的GaN层(10);以及growing a second temperature-stabilized GaN layer (10) on the GaN layer (9) grown at reduced temperature; and 在第二稳温生长的GaN层(10)上生长第二GaN覆盖层(11),形成一InGaN/GaN多量子阱。A second GaN cladding layer (11) is grown on the second temperature-stabilized GaN layer (10) to form an InGaN/GaN multi-quantum well. 2.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述MQW应力释放层(3)采用的是InGaN与GaN的超晶格结构,包括m个铟镓氮(InyGa1-yN)量子阱与m+1个氮化镓(GaN)量子势垒,每个InyGa1-yN量子阱上下两侧都有一个GaN量子垒,其中m≥1,0≤y≤1;GaN的厚度在之间,InGaN的厚度在之间。2. the method for growing high-quality InGaN/GaN multiple quantum wells without interruption according to claim 1, is characterized in that, what described MQW stress release layer (3) adopted is the superlattice structure of InGaN and GaN, comprises m Indium gallium nitride (In y Ga 1-y N) quantum wells and m+1 gallium nitride (GaN) quantum barriers, each In y Ga 1-y N quantum well has a GaN quantum barrier on the upper and lower sides , where m≥1, 0≤y≤1; the thickness of GaN is in arrive Between, the thickness of InGaN is in arrive between. 3.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述在MQW应力释放层(3)上外延生长InGaN量子阱(4),选用高纯N2做载气,厚度在之间,量子阱生长温度(QW_T)在750℃~900℃之间,In组分在0%~50%之间,选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。3. The method for growing high-quality InGaN/GaN multiple quantum wells without interruption according to claim 1, characterized in that, the epitaxial growth InGaN quantum wells (4) on the MQW stress release layer (3) is selected from high-purity N 2 as carrier gas, the thickness is Between, the quantum well growth temperature (QW_T) is between 750°C and 900°C, the In composition is between 0% and 50%, and SiH 4 is selected for n-type doping, and the doping concentration is between 1.0E+17cm - Between 3 and 5.0E+19cm -3 . 4.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述在InGaN量子阱(4)上生长第一GaN覆盖层(5),选用高纯N2做载气,厚度在之间,生长温度在750℃~900℃之间,选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。4. the method for growing high-quality InGaN/GaN multiple quantum wells without interruption according to claim 1, is characterized in that, the first GaN capping layer (5) of described growth on InGaN quantum well (4), selects high-purity N 2 as carrier gas, the thickness is Between, the growth temperature is between 750°C and 900°C, SiH 4 is selected for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 . 5.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述在第一GaN覆盖层(5)上生长升温生长的GaN层(6),选用GaN材料,同时通入高纯N2和高纯H2混合气做载气,N2和H2比例:1=<N2/H2<=100,三乙基镓(TEGa)作为镓源,厚度在之间,生长过程中温度始终处于变化的状态,温度从开始的量子阱生长温度一直上升到量子垒生长温度(QB_T),量子垒生长温度在800℃~1000℃之间,比量子阱生长温度高40℃以上;选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。5. the method for growing high-quality InGaN/GaN multiple quantum wells without discontinuity according to claim 1, is characterized in that, the GaN layer (6) of described growth temperature rise growth on the first GaN capping layer (5), selects For GaN materials, high-purity N 2 and high-purity H 2 mixed gas are introduced at the same time as the carrier gas, the ratio of N 2 and H2: 1=<N 2 /H 2 <=100, triethylgallium (TEGa) as the gallium source, thickness in During the growth process, the temperature is always in a state of change. The temperature rises from the initial quantum well growth temperature to the quantum barrier growth temperature (QB_T). Higher than 40°C; choose SiH 4 for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 . 6.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述在升温生长的GaN层(6)上生长第一稳温生长的GaN层(7),选用GaN材料,高纯N2和高纯H2混合气体做载气,N2和H2比例:1=<N2/H2<=100,生长过程中设定温度始终保持在量子垒生长温度,时间持续在10s~600s;选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。6. the method for growing high-quality InGaN/GaN multiple quantum wells without discontinuity according to claim 1, is characterized in that, the GaN layer (7) of the first temperature-stabilized growth is grown on the GaN layer (6) of temperature-raising growth ), choose GaN material, high-purity N 2 and high-purity H 2 mixed gas as the carrier gas, the ratio of N 2 and H 2 : 1=<N 2 /H 2 <=100, the set temperature during the growth process is always kept at the quantum The barrier growth temperature lasts from 10s to 600s; SiH 4 is selected for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 . 7.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述在第一稳温生长的GaN层(7)上生长GaN量子垒(8),选择GaN材料,同时通入高纯N2和高纯H2混合气做载气,N2和H2比例:1=<N2/H2<=100,厚度在之间,生长温度保持在量子垒生长温度;选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。7. The method for growing high-quality InGaN/GaN multiple quantum wells without interruption according to claim 1, characterized in that, the GaN quantum barrier (8) is grown on the GaN layer (7) of the first stable temperature growth, Choose GaN material, and feed high-purity N 2 and high-purity H 2 mixed gas as carrier gas at the same time, the ratio of N 2 and H 2 : 1=<N 2 /H 2 <=100, the thickness is at arrive In between, the growth temperature is maintained at the quantum barrier growth temperature; SiH 4 is selected for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 . 8.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述在GaN量子垒(8)上生长降温生长的GaN层(9),选择GaN材料,同时通入高纯N2和高纯H2混合气体做载气,N2和H2比例:1=<N2/H2<=100,厚度在之间,生长温度从量子垒生长温度下降到量子阱生长温度;选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。8. The method for growing high-quality InGaN/GaN multiple quantum wells without discontinuity according to claim 1, characterized in that, the GaN layer (9) grown on the GaN quantum barrier (8) is grown at a lower temperature, and the GaN material is selected , while feeding high-purity N 2 and high-purity H 2 mixed gas as carrier gas, the ratio of N 2 and H 2 : 1=<N 2 /H 2 <=100, the thickness is at arrive In between, the growth temperature drops from the quantum barrier growth temperature to the quantum well growth temperature; SiH 4 is selected for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 . 9.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述在降温生长的GaN层(9)上生长第二稳温生长的GaN层(10),选用GaN材料,同时通入高纯N2和高纯H2混合气体做载气,N2和H2比例:1=<N2/H2<=100,厚度在之间,生长温度保持在量子阱生长温度,时间持续在10s~600s;选用SiH4进行n型掺杂,掺杂浓度介于1.0E+17cm-3和5.0E+19cm-3之间。9. the method for growing high-quality InGaN/GaN multiple quantum wells without discontinuity according to claim 1, is characterized in that, the GaN layer (10) of the second stable temperature growth of described growth on the GaN layer (9) of cooling growth ), choose GaN material, and feed high-purity N 2 and high-purity H 2 mixed gas as carrier gas at the same time, the ratio of N 2 and H 2 : 1=<N 2 /H 2 <=100, the thickness is at arrive In between, the growth temperature is kept at the quantum well growth temperature, and the time lasts from 10s to 600s; SiH 4 is selected for n-type doping, and the doping concentration is between 1.0E+17cm -3 and 5.0E+19cm -3 . 10.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述在第二稳温生长的GaN层(10)上生长第二GaN覆盖层(11),采用高纯N2做载气,厚度在之间,生长温度与量子阱生长温度相同。10. the method for growing high-quality InGaN/GaN multiple quantum wells without interruption according to claim 1, is characterized in that, the second GaN capping layer (11) is grown on the GaN layer (10) of the second stable temperature growth ), using high-purity N 2 as carrier gas, with a thickness of Between, the growth temperature is the same as the quantum well growth temperature. 11.根据权利要求1所述的无间断生长高质量InGaN/GaN多量子阱的方法,其特征在于,所述在InGaN/GaN多量子阱上重复生长多个InGaN/GaN多量子阱,InGaN/GaN多量子阱的个数为N,且1=<N<=25。11. The method for growing high-quality InGaN/GaN multiple quantum wells without interruption according to claim 1, characterized in that, repeatedly growing a plurality of InGaN/GaN multiple quantum wells on the InGaN/GaN multiple quantum wells, InGaN/GaN multiple quantum wells The number of GaN multiple quantum wells is N, and 1=<N<=25.
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