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CN104600162B - 基于lao衬底的非极性蓝光led外延片的制备方法 - Google Patents

基于lao衬底的非极性蓝光led外延片的制备方法 Download PDF

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CN104600162B
CN104600162B CN201410112151.6A CN201410112151A CN104600162B CN 104600162 B CN104600162 B CN 104600162B CN 201410112151 A CN201410112151 A CN 201410112151A CN 104600162 B CN104600162 B CN 104600162B
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lao substrate
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CN104600162A (zh
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蔡卓然
高海
刘智
尹祥麟
刘正伟
张欣瑶
周环宇
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Shanghai Xi Xin Semiconductor Technology Co ltd
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Shanghai Chiptek Semiconductor Technology Co ltd
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Priority to PCT/CN2015/074828 priority patent/WO2015144023A1/zh
Priority to US15/128,639 priority patent/US9978908B2/en
Priority to PL15769396T priority patent/PL3107128T3/pl
Priority to RU2016138668A priority patent/RU2643176C1/ru
Priority to EP15769396.1A priority patent/EP3107128B1/en
Priority to JP2016574326A priority patent/JP6326154B2/ja
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Abstract

本发明公开了一种基于LAO衬底的非极性蓝光LED外延片及其制备方法，包括如下步骤：a)采用LAO衬底，选取晶体取向，并对LAO衬底进行表面清洁处理；b)对LAO衬底进行退火处理，并在LAO衬底表面形成AlN籽晶层；c)在LAO衬底上采用金属有机化合物化学气相淀积依次形成非极性m面GaN缓冲层、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、非极性m面AlGaN电子阻挡层和非极性p型掺杂GaN薄膜。本发明提供的基于LAO衬底的非极性蓝光LED外延片及其制备方法，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。

Description

基于LAO衬底的非极性蓝光LED外延片的制备方法
技术领域
本发明涉及一种LED外延片及其制备方法，尤其涉及一种基于LAO衬底的非极性蓝光LED外延片及其制备方法。
背景技术
目前LED蓝光外延片衬底主要为蓝宝石。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。
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‐confinedStarkerEffect，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。
发明内容
本发明所要解决的技术问题是提供一种基于LAO衬底的非极性蓝光LED外延片及其制备方法，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。
本发明为解决上述技术问题而采用的技术方案是提供一种基于LAO衬底的非极性蓝光LED外延片，包括衬底，其中，所述衬底为LAO衬底，所述LAO衬底上依次设置有缓冲层、第一非掺杂层、第一掺杂层、量子阱层、电子阻挡层和第二掺杂层。
上述的基于LAO衬底的非极性蓝光LED外延片，其中，所述缓冲层为非极性m面GaN缓冲层，所述第一非掺杂层为非极性非掺杂u‐GaN层，所述第一掺杂层为非极性n型掺杂GaN薄膜，所述量子阱层为非极性InGaN/GaN量子阱层，所述电子阻挡层为非极性m面AlGaN电子阻挡层，所述第二掺杂层为非极性p型掺杂GaN薄膜。
本发明为解决上述技术问题海提供一种基于LAO衬底的非极性蓝光LED外延片的制备方法，包括如下步骤：a)采用LAO衬底，选取晶体取向，并对LAO衬底进行表面清洁处理；b)对LAO衬底进行退火处理，并在LAO衬底表面形成AlN籽晶层；c)在LAO衬底上采用金属有机化合物化学气相淀积依次形成非极性m面GaN缓冲层、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、非极性m面AlGaN电子阻挡层和非极性p型掺杂GaN薄膜。
上述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其中，所述步骤b)包括如下过程：将LAO衬底在900～1200℃下高温烘烤1～4小时后空冷至室温，然后通入N2等离子体保温30～80分钟，在LAO衬底表面采用射频等离子体增强有机金属化学气相淀积形成AlN籽晶层，N等离子体的流量为40～90sccm，产生等离子体氮的射频功率为200～500W。
上述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其中，所述步骤c)中非极性m面GaN缓冲层的形成过程如下：将LAO衬底温度降为400～800℃，通入TMGa与N等离子体，控制反应室压力为400～700torr、N等离子体的流量为40～90sccm，产生等离子体氮的射频功率为200～700W，Ⅴ/Ⅲ比为800～1200。
上述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其中，所述步骤c)中非极性非掺杂u‐GaN层的形成过程如下：控制LAO衬底温度为1000～1500℃，通入TMGa，控制反应室压力为400torr，Ⅴ/Ⅲ比为180。
上述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其中，所述步骤c)中非极性n型掺杂GaN薄膜的形成过程如下：控制LAO衬底温度为1000～1300℃，通入TMGa和SiH4，保持SiH4的流量为60～100sccm，控制反应室压力为240torr，Ⅴ/Ⅲ比为160，掺杂电子浓度为1.0×1017～5.3×1019cm‐3；
上述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其中，所述步骤c)中非极性InGaN/GaN量子阱的形成过程如下：
形成垒层：控制LAO衬底温度为750～950℃，关闭H2，通入TEGa与氨气，控制反应室压力为200torr，Ⅴ/Ⅲ比为986，厚度为10～15nm；
形成阱层，控制LAO衬底温度为750～950℃，关闭H2，通入TEGa、TMIn与氨气，控制反应室压力为200torr，Ⅴ/Ⅲ比为1439，厚度为2～4nm。
上述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其中，所述步骤c)中非极性m面AlGaN电子阻挡层的形成过程如下：将LAO衬底温度升至900～1050℃，通入TMGa与氨气，控制反应室压力为200torr，Ⅴ/Ⅲ比为986。
上述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其中，所述步骤c)中非极性p型掺杂GaN薄膜的形成过程如下：控制LAO衬底温度为900～1100℃，通入TMGa、CP2Mg与氨气，保持CP2Mg的流量为250～450sccm，控制反应室压力为200torr，Ⅴ/Ⅲ比为1000～1250，掺杂空穴浓度1.0×1016～2.2×1018cm‐3。
本发明对比现有技术有如下的有益效果：本发明提供的基于LAO衬底的非极性蓝光LED外延片及其制备方法，通过采用LAO衬底，并在LAO衬底上依次设置缓冲层、第一非掺杂层、第一掺杂层、量子阱层、电子阻挡层和第二掺杂层，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。
附图说明
图1为本发明基于LAO衬底的非极性蓝光LED外延片结构示意图；
图2为本发明的用于LAO衬底的非极性蓝光LED外延片的制备装置结构示意图；
图3为本发明基于LAO衬底的非极性蓝光LED外延片制备流程示意图；
图4为本发明生长在LAO衬底(001)面上的非极性蓝光LED外延片的XRD测试图；
图5为本发明生长在LAO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；
图6为本发明生长在LAO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。
具体实施方式
下面结合附图和实施例对本发明作进一步的描述。
图1为本发明基于LAO衬底的非极性蓝光LED外延片结构示意图。
请参见图1，本发明提供的基于LAO衬底的非极性蓝光LED外延片，包括衬底，其中，所述衬底为LAO衬底，所述LAO衬底上依次设置有缓冲层、第一非掺杂层、第一掺杂层、量子阱层、电子阻挡层和第二掺杂层。本发明的生长在LAO衬底上的非极性蓝光LED外延片，所述LAO衬底又称镧铝氧化物衬底，由La,Al,O元素组成，分子式为LaAlxOy。如图1所示，本发明提供的非极性蓝光LED外延片包括由下至上依次排列的LAO衬底10、非极性m面GaN缓冲层11、非极性非掺杂u‐GaN层12、非极性n型掺杂GaN薄膜13、非极性InGaN/GaN量子阱层14、非极性m面AlGaN电子阻挡层15、非极性p型掺杂GaN薄膜16。
图2为本发明的用于LAO衬底的非极性蓝光LED外延片的制备装置结构示意图。
请继续参见图2，20、21分别为NH3和SiH4，其作用是提供N和Si；22是H2,其作用是作为载气，输送Cp2Mg、TMGa、TMIn；23、24、25分别是Cp2Mg、TMGa、TMIn，其作用是提供LED生长所需的Mg、Ga、In；26是机械手，用于输送衬底和样品；27是射频感应加热器，用来对衬底加热及控温；28是石墨盘，用于承载LAO衬底；29是反应腔，各种反应气体发生化学反应生成LED的腔体；30是喷头，反应气体充分混合后均匀喷射到衬底表面的装置；31是射频等离子源装置，用于提供活性N；32‐40是阀门，用于控制各种管道的气体的输送状态。MFC是流量控制器，用于控制气体的流量，从而满足生长的需求。
图3为本发明基于LAO衬底的非极性蓝光LED外延片制备流程示意图。
请继续参见图3，本发明的生长在LAO衬底上的非极性蓝光LED外延片的制备方法，具体包括以下步骤：
步骤S1：采用LAO衬底，选取晶体取向，并对LAO衬底进行表面清洁处理；
步骤S2：对LAO衬底进行退火处理，并在LAO衬底表面形成AlN籽晶层；
步骤S3：在LAO衬底上采用金属有机化合物化学气相淀积依次形成非极性m面GaN缓冲层、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、非极性m面AlGaN电子阻挡层和非极性p型掺杂GaN薄膜。
下面给出一个具体实施例，制作步骤及工艺条件如下：
(1)采用LAO衬底，选取晶体取向；
(2)对衬底进行表面清洁处理；
(3)对衬底进行退火处理：将衬底在900‐1200℃下高温烘烤1～4h后空冷至室温，然后通入N2等离子体保温30～80分钟，在衬底表面形成AlN籽晶层，为GaN薄膜的生长提供模板，N等离子体的流量为40～90sccm，产生等离子体氮的射频功率为200～500W；
(4)采用射频等离子体(RF)增强有机金属化学气相淀积(MOCVD)生长非极性m面GaN缓冲层，工艺条件为：将衬底温度降为400～800℃，通入TMGa与N等离子体，反应室压力为400～700torr、N等离子体的流量为40～90sccm，产生等离子体氮的射频功率为200～700W，Ⅴ/Ⅲ比为800～1200；
(5)采用MOCVD工艺生长非极性非掺杂u‐GaN层，工艺条件为：衬底温度为1000～1500℃，通入TMGa，反应室压力为400torr，Ⅴ/Ⅲ比为180；
(6)采用MOCVD工艺生长非极性n型掺杂GaN薄膜，工艺条件为：衬底温度为1000～1300℃，通入TMGa和SiH4，保持SiH4的流量为60～100sccm，反应室压力为240torr，Ⅴ/Ⅲ比为160；掺杂电子浓度1.0×1017～5.3×1019cm‐3；
(7)采用MOCVD工艺生长非极性InGaN/GaN量子阱，工艺条件为：形成垒层，衬底温度为750～950℃，关闭H2，通入TEGa与氨气，反应室压力为200torr，Ⅴ/Ⅲ比为986，厚度为10～15nm；形成阱层，衬底温度为750～950℃，关闭H2，通入TEGa、TMIn与氨气，反应室压力为200torr，Ⅴ/Ⅲ比为1439，厚度为2～4nm；
(8)采用MOCVD工艺生长非极性m面AlGaN电子阻挡层，工艺条件为：衬底温度升至900～1050℃，通入TMGa与氨气，反应室压力为200torr，Ⅴ/Ⅲ比为986；
(9)采用MOCVD工艺生长非极性p型掺杂GaN薄膜，工艺条件为：衬底温度为900～1100℃，通入TMGa、CP2Mg与氨气，保持CP2Mg的流量为250～450sccm，反应室压力为200torr，Ⅴ/Ⅲ比为1000～1250；掺杂空穴浓度1.0×1016‐2.2×1018cm‐3。
图4为本发明生长在LAO衬底(001)面上的非极性蓝光LED外延片的XRD测试图。
由图4可见，本发明测试得到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°，表明本发明制备的非极性蓝光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。
图5为本发明生长在LAO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5可见，本发明温度为293K下PL谱测试得到发光峰波长为460nm，半峰宽为23nm。这表明本发明制备的非极性GaN薄膜在光学性质上具有非常好的性能。
图6为本发明生长在LAO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6可见，温度为293K下EL谱测试得到发光峰波长为461nm，半峰宽为22nm，输出功率为7.8mw20mA。表明本发明制备的非极性GaN薄膜在电学性质上具有非常好的性能。
综上所述，本发明提供的基于LAO衬底的非极性蓝光LED外延片及其制备方法，通过采用LAO衬底，并在LAO衬底上依次设置非极性m面GaN缓冲层、非极性非掺杂GaN层、非极性n型掺杂GaN薄膜、非极性InGaN/GaN量子阱层、非极性m面AlGaN电子阻挡层和非极性p型掺杂GaN薄膜。与现有技术相比，本发明具有生长工艺简单，制备成本低廉的优点，且制备的非极性蓝光LED外延片缺陷密度低、结晶质量好，电学、光学性能好。
虽然本发明已以较佳实施例揭示如上，然其并非用以限定本发明，任何本领域技术人员，在不脱离本发明的精神和范围内，当可作些许的修改和完善，因此本发明的保护范围当以权利要求书所界定的为准。

Claims (8)

1.一种基于LAO衬底的非极性蓝光LED外延片的制备方法，所述LED外延片包括衬底，所述衬底为LAO衬底，所述LAO衬底上依次设置有缓冲层、第一非掺杂层、第一掺杂层、量子阱层、电子阻挡层和第二掺杂层，所述缓冲层为非极性m面GaN缓冲层，所述第一非掺杂层为非极性非掺杂u-GaN层，所述第一掺杂层为非极性n型掺杂GaN薄膜，所述量子阱层为非极性InGaN/GaN量子阱层，所述电子阻挡层为非极性m面AlGaN电子阻挡层，所述第二掺杂层为非极性p型掺杂GaN薄膜；其特征在于，所述制备方法包括如下步骤：
a)采用LAO衬底，选取晶体取向，并对LAO衬底进行表面清洁处理；
b)对LAO衬底进行退火处理，并在LAO衬底表面形成AlN籽晶层；
c)在LAO衬底上采用金属有机化合物化学气相淀积依次形成非极性m面GaN缓冲层、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、非极性m面AlGaN电子阻挡层和非极性p型掺杂GaN薄膜。
2.如权利要求1所述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其特征在于，所述步骤b)包括如下过程：
将LAO衬底在900～1200℃下高温烘烤1～4小时后空冷至室温，然后通入N2等离子体保温30～80分钟，在LAO衬底表面采用射频等离子体增强有机金属化学气相淀积形成AlN籽晶层，N等离子体的流量为40～90sccm，产生等离子体氮的射频功率为200～500W。
3.如权利要求1所述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其特征在于，所述步骤c)中非极性m面GaN缓冲层的形成过程如下：将LAO衬底温度降为400～800℃，通入TMGa与N等离子体，控制反应室压力为400～700torr、N等离子体的流量为40～90sccm，产生等离子体氮的射频功率为200～700W，Ⅴ/Ⅲ比为800～1200。
4.如权利要求1所述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其特征在于，所述步骤c)中非极性非掺杂u-GaN层的形成过程如下：控制LAO衬底温度为1000～1500℃，通入TMGa，控制反应室压力为400torr，Ⅴ/Ⅲ比为180。
5.如权利要求1所述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其特征在于，所述步骤c)中非极性n型掺杂GaN薄膜的形成过程如下：控制LAO衬底温度为1000～1300℃，通入TMGa和SiH4，保持SiH4的流量为60～100sccm，控制反应室压力为240torr，Ⅴ/Ⅲ比为160，掺杂电子浓度为1.0×1017～5.3×1019cm-3。
6.如权利要求1所述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其特征在于，所述步骤c)中非极性InGaN/GaN量子阱的形成过程如下：
形成垒层：控制LAO衬底温度为750～950℃，关闭H2，通入TEGa与氨气，控制反应室压力为200torr，Ⅴ/Ⅲ比为986，厚度为10～15nm；
形成阱层，控制LAO衬底温度为750～950℃，关闭H2，通入TEGa、TMIn与氨气，控制反应室压力为200torr，Ⅴ/Ⅲ比为1439，厚度为2～4nm。
7.如权利要求1所述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其特征在于，所述步骤c)中非极性m面AlGaN电子阻挡层的形成过程如下：将LAO衬底温度升至900～1050℃，通入TMGa与氨气，控制反应室压力为200torr，Ⅴ/Ⅲ比为986。
8.如权利要求1所述的基于LAO衬底的非极性蓝光LED外延片的制备方法，其特征在于，所述步骤c)中非极性p型掺杂GaN薄膜的形成过程如下：控制LAO衬底温度为900～1100℃，通入TMGa、CP2Mg与氨气，保持CP2Mg的流量为250～450sccm，控制反应室压力为200torr，Ⅴ/Ⅲ比为1000～1250，掺杂空穴浓度1.0×1016～2.2×1018cm-3。
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