CN104037285A - 一种生长在Si衬底上的GaN薄膜及其制备方法和应用 - Google Patents

一种生长在Si衬底上的GaN薄膜及其制备方法和应用 Download PDF

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CN104037285A
CN104037285A CN201410256444.1A CN201410256444A CN104037285A CN 104037285 A CN104037285 A CN 104037285A CN 201410256444 A CN201410256444 A CN 201410256444A CN 104037285 A CN104037285 A CN 104037285A
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李国强
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Guangzhou Zhongtuo Optoelectrical Technology Co Ltd
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Abstract

本发明公开了一种生长在Si衬底上的GaN薄膜，其包括由下至上依次排列的Si衬底、AlN缓冲层、GaN形核层、GaN外延层；所述Si衬底的晶体取向为111面偏100方向0.5-1°；通过衬底以及其晶向的选取、采用脉冲激光沉积工艺生长AlN缓冲层、采用金属有机化学气相沉积工艺生长GaN形核层、采用金属有机化学气相沉积工艺生长GaN外延层等步骤制备而成。本发明的GaN薄膜应用于LED器件、光电探测器等器件中，具有密度低、结晶质量好、成本低等优点。

Description

一种生长在Si衬底上的GaN薄膜及其制备方法和应用
技术领域
本发明涉及金属有机化学气相沉积法合成膜的技术领域，具体涉及一种生长在Si衬底上的GaN薄膜及其制备方法和应用。
背景技术
GaN作为第三代半导体材料代表之一，具有直接带隙、宽禁带、高饱和电子漂移速度、高击穿电场和高热导率等优异性能，在微电子应用方面也得到了广泛的关注。自I.Akasaki首次成功获得p-GaN，实现蓝光LED的新突破后，GaN基化合物半导体一直备受关注，在室内照明、商业照明、工程照明等领域有着广泛的应用。
高质量GaN材料一般都通过异质外延方法制作。作为常用于生长GaN的衬底，蓝宝石有稳定的物理化学性质，但它与GaN间存在很大的晶格失配(16％)及热失配(25％)，造成生长的GaN外延层质量较差；SiC虽然与GaN的晶格失配度仅3.5％，导热率较高，但它的热失配与蓝宝石相当(25.6％)，与GaN的润湿性较差，价格昂贵，并且制造技术已被美国科锐公司垄断，因此也无法普遍使用。相比较下，Si衬底具有成本低、单晶尺寸大且质量高、导热率高、导电性能良好等诸多特点，并且Si的微电子技术十分成熟，在Si衬底上生长GaN薄膜有望实现光电子和微电子的集成。正是因为Si衬底的上述诸多优点，Si衬底上生长GaN薄膜进而制备LED越来越备受关注。但是，目前在Si衬底上制备GaN单晶薄膜的质量不如蓝宝石衬底，主要由于：Si与GaN热失配远远高于蓝宝石，导致外延片更易于龟裂；Si衬底遇活性N在界面处易形成无定形的SixNy，影响GaN的生长质量；Si对可见光的吸收作用也会大大降低LED发光效率。
由此可见，即便Si衬底具有成本低、散热好等优点，具有非常良好的发展前景，但要获得在Si衬底上生长高质量GaN薄膜，需要寻找Si衬底上生长GaN薄膜的新方法及工艺。
发明内容
为了克服现有技术的不足，本发明的目的在于提供一种生长在Si衬底上的GaN薄膜，具有密度低、结晶质量好、成本低等优点。
本发明的另一目的在于提供一种生长在Si衬底上的GaN薄膜的制备方法，以提高GaN薄膜的均匀性及生长速度，并降低成本。
本发明的第三个目的在于提供生长在Si衬底上的GaN薄膜在制备蓝光LED灯中的应用。
为解决上述问题，本发明所采用的技术方案如下：
一种生长在Si衬底上的GaN薄膜，其包括由下至上依次排列的Si衬底、AlN缓冲层、GaN形核层、GaN外延层；所述Si衬底的晶体取向为111面偏100方向0.5-1°。
在上述方案的基础上，优选的，本发明所述AlN缓冲层厚度为10-50nm。
在上述方案的基础上，优选的，本发明所述GaN形核层厚度为3-10nm。
在上述方案的基础上，优选的，本发明所述GaN外延层厚度为1.2-1.5μm。
上述生长在Si衬底上的GaN薄膜的制备方法，顺次包括以下步骤：
1)衬底以及其晶向的选取：采用Si衬底，选取111面偏100方向0.5-1°的晶体取向；
2)采用脉冲激光沉积工艺生长AlN缓冲层；
3)采用金属有机化学气相沉积工艺生长GaN形核层；
4)采用金属有机化学气相沉积工艺生长GaN外延层。
在上述方案的基础上，作为优选的，所述制备方法在步骤1)之后、步骤2)之前还包括了对衬底依次进行表面清洗和退火处理。其中所述表面清洗具体步骤为：对衬底进行表面清洁处理是将Si衬底放入丙酮溶液中超声处理，然后用去离子水清洗；接着在异丙酮溶液中超声处理；再在氢氟酸溶液中浸泡；然后放入去离子水中浸泡；最后在硫酸和双氧水的混合溶液中浸泡，再经氢氟酸浸泡，然后用去离子水冲洗，氮气吹干，存放于氮气柜中。所述退火处理是将衬底在900-1000℃下高温烘烤3-5h；通过退火处理使衬底获得原子级平整的表面，进一步提高了GaN薄膜的平整性和均匀性。
步骤4)中生长AlN缓冲层时，衬底温度为650-750℃，反应室压力为10-15mTorr、V/III比为50-60、生长速度为0.4-0.6ML/s。
步骤5)生长GaN形核层时，衬底温度为1000-1300℃，反应室压力为450-500Torr、V/III比为3000-3300、生长速度为0.8-1.0μm/h。
步骤6)中生长GaN外延层时，衬底温度升至1030-1060℃，反应室压力为150～220Torr，V/III为1000-1200，生长速率为3.0-3.5μm/h。
上述GaN薄膜在制备LED器件、光电探测器中的应用。
相比现有技术，本发明的有益效果在于：
采用金属有机化学气相沉积工艺与脉冲激光沉积工艺相结合，先采用脉冲激光沉积工艺生长AlN缓冲层，避开采用金属有机化学气相沉积工艺生长AlN所需经过的预铺Al工序，防止因预铺Al不均匀造成的AlN质量下降；再低温生长AlN缓冲层，防止Si在高温下扩散至AlN缓冲层破坏表面形貌，最后高温生长GaN外延层，以提高GaN薄膜的均匀性及生长速度。
下面结合附图和具体实施方式对本发明作进一步详细说明。
附图说明
图1为本发明的生长在Si衬底上的GaN薄膜截面示意图；
图2为本发明的生长在Si衬底上的GaN薄膜X射线面扫描谱图；
图3为本发明的生长在Si衬底上的GaN薄膜X射线回摆曲线图；
图4为本发明的生长在Si衬底上的GaN薄膜应用在LED器件中的示意图；
图5为本发明的生长在Si衬底上的GaN薄膜应用在太阳能电池中的示意图。
具体实施方式
实施例1
参照图1，本发明的生长在Si衬底上的GaN薄膜包括Si衬底11、AlN缓冲层12、GaN形核层13、GaN外延层14，
上述生长在Si衬底上的GaN薄膜顺次采用如下步骤获得：
(1)衬底及晶向的选择：采用Si衬底，选取111面偏100方向0.5°的晶体取向。
(2)采用脉冲激光沉积工艺生长AlN缓冲层，工艺条件为：衬底温度为650℃，反应室压力为15mTorr、V/III比为50、生长速度为0.4ML/s。
(3)采用金属有机化学气相沉积工艺生长GaN形核层，工艺条件为：衬底温度为1300℃，反应室压力为450Torr、V/III比为3000、生长速度为0.8μm/h。
(4)采用金属有机化学气相沉积工艺生长GaN外延层，工艺条件为：衬底温度升至1030℃，反应室压力为220Torr，V/III为1000，生长速率为3.0μm/h。
实施例2
参照图1，本发明的生长在Si衬底上的GaN薄膜包括Si衬底11、AlN缓冲层12、GaN形核层13、GaN外延层14，
上述生长在Si衬底上的GaN薄膜顺次采用如下步骤获得：
(1)衬底及晶向的选择：采用Si衬底，选取111面偏100方向1°的晶体取向。
(2)采用脉冲激光沉积工艺生长AlN缓冲层，工艺条件为：衬底温度为750℃，反应室压力为10mTorr、V/III比为60、生长速度为0.6ML/s。
(3)采用金属有机化学气相沉积工艺生长GaN形核层，工艺条件为：衬底温度为1000℃，反应室压力为450Torr、V/III比为3300、生长速度为1.0μm/h。
(4)采用金属有机化学气相沉积工艺生长GaN外延层，工艺条件为：衬底温度升至1060℃，反应室压力为150Torr，V/III为1200，生长速率为3.5μm/h。
实施例3
一种生长在Si衬底上的GaN薄膜顺次采用如下步骤获得：
1)衬底及晶向的选择：采用Si衬底，选取111面偏100方向0.5°的晶体取向。
2)表面清洗处理：将Si衬底先放在丙酮溶液中超声清洗，然后再放在去离子水中超声清洗；接着在异丙酮溶液中超声清洗；然后在氢氟酸溶液中超声清洗，再在去离子水中浸泡；再将Si衬底放在硫酸和双氧水的混合溶液中浸泡；最后将Si衬底放入氢氟酸中浸泡，用去离子水冲洗，氮气吹干。
3)退火处理：将衬底在900℃下高温烘烤5h。
4)采用脉冲激光沉积工艺生长AlN缓冲层，工艺条件为：衬底温度为650℃，反应室压力为15mTorr、V/III比为50、生长速度为0.4ML/s。
5)采用金属有机化学气相沉积工艺生长GaN形核层，工艺条件为：衬底温度为1300℃，反应室压力为450Torr、V/III比为3000、生长速度为0.8μm/h。
6)采用金属有机化学气相沉积工艺生长GaN外延层，工艺条件为：衬底温度升至1030℃，反应室压力为220Torr，V/III为1000，生长速率为3.0μm/h。
参照图2，从X射线面扫描图谱中可以看到，GaN薄膜成功在Si衬底行外延生长，外延关系为：GaN(002)//AlN(002)//Si(111)。
请参照图3，从X射线回摆曲线图中可以看到，GaN(002)薄膜的半峰宽(FWHM)值低于0.2°，表明在Si(111)面上外延生长出了低缺陷密度的高质量GaN薄膜。
实施例4
1)衬底及晶向的选择：采用Si衬底，选取(111)面偏(100)方向1°的晶体取向。
2)表面清洗处理：将Si衬底先放在丙酮溶液中超声清洗，然后再放在去离子水中超声清洗；接着在异丙酮溶液中超声清洗；然后在氢氟酸溶液中超声清洗，再在去离子水中浸泡；再将Si衬底放在硫酸和双氧水的混合溶液中浸泡；最后将Si衬底放入氢氟酸中浸泡，用去离子水冲洗，氮气吹干。
3)退火处理：将衬底在900℃下高温烘烤5h。
4)采用脉冲激光沉积工艺生长AlN缓冲层，工艺条件为：衬底温度为750℃，反应室压力为10mTorr、V/III比为60、生长速度为0.6ML/s。
5)采用金属有机化学气相沉积工艺生长GaN形核层，工艺条件为：衬底温度为1000℃，反应室压力为450Torr、V/III比为3300、生长速度为1.0μm/h。
6)采用金属有机化学气相沉积工艺生长GaN外延层，工艺条件为：衬底温度升至1060℃，反应室压力为150Torr，V/III为1200，生长速率为3.5μm/h。
应用实施例1：生长在Si衬底上的GaN薄膜在LED器件中的应用
参照图4，将实施例3获得的GaN薄膜应用到LED器件中的方法，其包括在Si(111)晶面上外延生长高质量GaN薄膜20后，依次生长高质量的n型掺硅GaN外延层21,InxGa1-xN多量子阱层22，p型掺镁GaN层23，具体如下：
在GaN薄膜层10上生长n型掺硅GaN外延层21,其厚度约为3μm，其载流子的浓度为1×1019cm-3，接着生长InxGa1-xN多量子阱层22,厚度约为112nm,周期数为7，其中InxGa1-xN阱层为3nm，垒层为13nm，0＜x＜1；之后再生长p型掺镁GaN层23,厚度约为350nm，其载流子浓度为2×1016cm-3；最后电子束蒸发形成欧姆接触；在此基础上通过在N2气氛下退火，提高p型掺镁GaN层23的载流子浓度和迁移率。
应用实施例2：生长在Si衬底上的GaN薄膜在太阳能电池中的应用
参照图5，将实施例4获得的生长在Si衬底上的GaN薄膜应用在太阳能电池中，方法是：在Si(111)晶面上外延生长高质量的GaN薄膜层30后，再生长具有成分梯度的InxGa1-xN缓冲层31、n型掺硅InxGa1-xN层32、InxGa1-xN多量子阱层33、p型掺镁InxGa1-xN层34，获得含长在Si衬底上的GaN薄膜的电器元件，具体过程如下：
在GaN薄膜层30上生长高质量的具有成分梯度的InxGa1-xN缓冲层31，其x的值可以在0-0.2之间可调；然后生长n型掺硅InxGa1-xN层32，其厚度约为5μm，其载流子的浓度为1×1019cm-3，0＜x＜1。接着生长InxGa1-xN多量子阱层33，厚度约为300nm，周期数为20，0＜x＜1，其中In0.2Ga0.8N阱层为3nm，In0.08Ga0.92N垒层为10nm。再生长Mg掺杂的p型掺镁InxGa1-xN层34，厚度约为200nm，0＜x＜1，其载流子浓度为2×1016cm-3。最后电子束蒸发形成欧姆接触。在此基础上通过在N2气氛下退火，提高了p型掺镁InxGa1-xN层34的载流子浓度和迁移率。
上述实施方式仅为本发明的优选实施方式，不能以此来限定本发明保护的范围，本领域的技术人员在本发明的基础上所做的任何非实质性的变化及替换均属于本发明所要求保护的范围。

Claims (10)

1.一种生长在Si衬底上的GaN薄膜，其特征在于：其包括由下至上依次排列的Si衬底、AlN缓冲层、GaN形核层、GaN外延层；所述Si衬底的晶体取向为111面偏100方向0.5-1°。
2.根据权利要求1所述的GaN薄膜，其特征在于：所述AlN缓冲层厚度为10-50nm；所述GaN形核层厚度为3-10nm；所述GaN外延层厚度为1.2-1.5μm。
3.如权利要求1所述的生长在Si衬底上的GaN薄膜的制备方法，顺次包括以下步骤：
1)衬底以及其晶向的选取：采用Si衬底，选取111面偏100方向0.5-1°的晶体取向；
2)采用脉冲激光沉积工艺生长AlN缓冲层；
3)采用金属有机化学气相沉积工艺生长GaN形核层；
4)采用金属有机化学气相沉积工艺生长GaN外延层。
4.根据权利要求3所述的制备方法，其特征在于：在步骤1)之后、步骤2)之前还包括了对衬底依次进行表面清洗和退火处理。
5.根据权利要求4所述的制备方法，其特征在于，所述表面清洗具体步骤为：对衬底进行表面清洁处理是将Si衬底放入丙酮溶液中超声处理，然后用去离子水清洗；接着在异丙酮溶液中超声处理后，在氢氟酸溶液中浸泡；然后放入去离子水中浸泡；最后在硫酸和双氧水的混合溶液中浸泡，再经氢氟酸浸泡，然后用去离子水冲洗，氮气吹干，存放于氮气柜中。
6.根据权利要求4所述的制备方法，其特征在于，所述退火处理是将衬底在900-1000℃下高温烘烤3-5h。
7.根据权利要求3或4所述的制备方法，其特征在于：步骤2)中生长AlN缓冲层时，衬底温度为650-750℃，反应室压力为10-15mTorr、V/III比为50-60、生长速度为0.4-0.6ML/s。
8.根据权利要求3或4所述的制备方法，其特征在于：步骤3)生长GaN形核层时，衬底温度为1000-1300℃，反应室压力为450-500Torr、V/III比为3000-3300、生长速度为0.8-1.0μm/h。
9.根据权利要求3或4所述的制备方法，其特征在于：步骤4)中生长GaN外延层时，衬底温度升至1030-1060℃，反应室压力为150～220Torr，V/III为1000-1200，生长速率为3.0-3.5μm/h。
10.如权利要求1或2所述的GaN薄膜在制备LED器件、光电探测器中的应用。
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