CN1702836A - 非极性单晶a－面氮化物半导体晶圆及其制备 - Google Patents

非极性单晶a－面氮化物半导体晶圆及其制备 Download PDF

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CN1702836A
CN1702836A CNA200510071276XA CN200510071276A CN1702836A CN 1702836 A CN1702836 A CN 1702836A CN A200510071276X A CNA200510071276X A CN A200510071276XA CN 200510071276 A CN200510071276 A CN 200510071276A CN 1702836 A CN1702836 A CN 1702836A
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申铉敏
李惠龙
李昌浩
金贤锡
金政敦
孔善焕
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Corning Precision Materials Co Ltd
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Abstract

在950到1100℃的温度范围内并且以30到300μm/hr的速度在单晶r－面蓝宝石衬底上氢化物气相外延(HVPE)生长a－面氮化物半导体膜，可以快速且有效地制备无空隙、翘曲或裂纹的单晶a－面氮化物半导体晶圆。

Description

非极性单晶A-面氮化物半导体晶圆及其制备
技术领域
本发明涉及一种无空隙、翘曲或裂纹的非极性单晶a-面氮化物半导体晶圆以及用于制备所述的氮化物半导体晶圆的方法。
背景技术
在制造半导体器件中用作衬底的单晶氮化物基晶圆主要是通过常规方法在c-面蓝宝石衬底上生长、然后与其分离的c-面({0001}面)薄膜，所述常规方法，例如，金属有机化学气相淀积(MOCVD)、分子束外延(MBE)和氢化物气相外延(HVPE)。
然而，这种在c-面蓝宝石衬底上生长的c-面氮化物膜由于在生长期间界面处的晶格参数和热膨胀系数的不同而易于产生裂纹。在c-面氮化物膜掺杂有诸如硅的元素的情况下，该裂纹问题就更加严重。还有，c-面氮化物膜，例如在c-面蓝宝石或(0001)SiC衬底之上的GaN/AlGaN异质结构，具有沿着纤维锌矿晶体结构的极性c-轴的自发或压电极化场。这些极化的不连续在相邻器件层之间的界面处产生导致内部电场的固定表面电荷。这些极性-感应电场在量子阱结构中在空间上分离电子和空穴波函数，由此减少了内部量子效率并且显著地改变了器件的电子特性和光学特性。
与c-面氮化物膜相反，在r-面({1-102}面)蓝宝石衬底上生长的a-面({11-20}面)氮化物膜是非极性的，这样没有展示出极化场和量子限制斯塔克效应，并且可以有利于用作高效发光二极管和大功率微波晶体管。
然而，当在r-面衬底上生长a-面氮化物膜时，它获得了向<0001>方向(参见图1)延伸的具有{1010}-面脊的非平坦表面形态和由于缺少这些脊的聚结而产生的内部宏空隙，由于上述原因，所以在商业上仍然得不到这种a-面氮化物膜衬底。上述表面的不规则性和宏缺陷限制了多层器件的制造和性能。
美国专利公开No.2003-198837公开了一种通过在a-面氮化镓(GaN)膜的高温生长之前形成具有100nm厚度的低温GaN缓冲层而在r-面蓝宝石衬底上生长具有平坦表面的1.5μm厚的a-面GaN膜的方法，其中所述a-面GaN膜的高温生长是通过MOCVD在低压下进行。然而，这种方法不适用于形成30μm或更厚的厚膜，其用作独立的衬底。
发明内容
相应地，本发明的一个目的是提供一种无空隙、翘曲或裂纹的高质量的非极性单晶a-面氮化物半导体晶圆。
本发明的另一个目的是提供一种用于制备所述氮化物半导体晶圆的有效方法。
根据本发明的一个方案，提供一种通过在单晶r-面蓝宝石衬底上进行氢化物气相外延(HVPE)而获得的130μm或更厚的单晶a-面氮化物半导体晶圆。
根据本发明的另一个方案，提供一种用于制备单晶a-面氮化物半导体晶圆的方法，该方法包括：通过氢化物气相外延(HVPE)，以30到300μm/hr速度在加热至从950到1100℃的温度范围的单晶r-面蓝宝石衬底上生长a-面氮化物膜，从衬底分离生长的a-面氮化物膜，以及抛光其表面。
附图说明
当结合附图，从对本发明进行的以下说明中，本发明的上述和其他目的和特点将会变得显而易见，所述附图分别示出：
图1：示出在单晶r-面蓝宝石衬底上的单晶a-面氮化物厚膜的异质外延生长的情况下的晶格参数的差异与生长的氮化物膜的类脊表面形态的示意图；
图2：根据本发明方法的一个优选实施例的用于制备单晶a-面氮化物晶圆的步骤；
图3：根据本发明方法在蓝宝石衬底上生长单晶a-面氮化物厚膜时在r-面蓝宝石衬底之内产生的微裂纹；
图4和5：在实施例1中分别获得的a-面GaN厚膜(抛光之前)的照片和X射线衍射(XRD)图形；
图6：在实施例1中获得的a-面GaN厚膜(在分离和抛光之后)的照片；
图7A和7B：在实施例1中分别获得的a-面GaN厚膜(在抛光之前)表面的扫描电子显微镜(SEM)照片和XRD振动曲线；以及
图8A和8B：在实施例2中分别获得的a-面GaN厚膜(在抛光之前)表面的SEM照片和XRD振动曲线。
11：单晶r-面蓝宝石衬底
12：氮化的r-面蓝宝石衬底表面
13：单晶a-面氮化物半导体薄膜
14：单晶a-面氮化物半导体厚膜
20：抛光的独立的a-面氮化物半导体晶圆
发明详述
本发明的特征在于，通过由HVPE、在950到1100℃的温度范围下、以30-300μm/hr速度、在r-面蓝宝石衬底上生长氮化物半导体膜，来制备无空隙、翘曲或裂纹的非极性单晶a-面氮化物半导体晶圆。
图2说明了根据本发明方法的一个优选实施例的用于制备作为独立的基板的单晶a-面氮化物晶圆的一系列步骤，所述步骤包括：(a)制备单晶r-面蓝宝石衬底(11)，(b)氮化蓝宝石衬底(11)的一个表面，(c)采用根据本发明方法的HVPE在衬底的已氮化表面(12)上生长单晶a-面氮化物半导体薄膜(13)，(d)连续生长氮化物膜(13)，以形成聚结的a-面氮化物半导体厚膜(14)，(e)从衬底(11)分离氮化物膜(14)，以及(f)抛光分离的氮化物膜的表面，以形成平坦的a-面氮化物半导体独立的基板(20)。
在衬底上生长的氮化物化合物半导体可以是选自由Ga、Al和In组成的组中的至少一种III族元素的氮化物，其由化学式[AlxGayIn1-x-yN](0≤x≤1，0≤y≤1，0≤x+y≤1)表示。除了蓝宝石(α-Al2O3)之外，可以采用诸如ZnO、Si、SiC、铝酸锂、硫镓铜矿锂(lithiumgallite)、GaAs和GaN等常规材料中的任何一种材料作为r-面衬底。
根据本发明的方法，可以经由使III族元素的氯化物蒸汽和气态的氨(NH3)与保持在950-1100℃的温度范围下的衬底表面接触，通过氢化物气相外延(HVPE)，以30到300μm/hr的生长速度、优选以30到200μm/hr的生长速度，在r-面蓝宝石衬底上生长a-面氮化物半导体膜。当生长温度低于950℃时，氮化物膜的结晶性变差，并且当其高于1100℃时，由于生长的氮化物晶体的分解，所以生长速度和结晶性变低。如果生长速度大于300μm/hr，那么因成分扩散到合适的晶格位置的时间不充分，还会观察到氮化物膜的结晶性退化。
通过在器皿上放置一种或多种III族元素并将气态的氯化氢(HCl)引入到其上，可以在HVPE反应器中产生III族元素的氯化物蒸汽。反应器腔可以在环境压力之下保持在600-900℃的温度范围内。按照1∶2～20、优选1∶2～5的体积比引入气态的氯化氢和氨。在前一种条件下提供的是在X射线衍射(XRD)振动曲线中具有1000弧度秒(arcsec)或更小的FWHM(半最高幅度的全宽度)值的a-面氮化物膜，并且在后一种条件下，获得具有500arcsec或更小的FWHM值的a-面氮化物膜。FWHM值的下降表示改善的结晶性。
如果必要，可以通过使氨(NH3)和氯化氢(HCl)的气体混合物在900到1100℃的温度范围下与r-面蓝宝石衬底的表面接触来氮化其。此外，为了提高氮化性，衬底表面可以在上述氮化步骤之前或之后进一步用气态的氨(NH3)来进行处理。可以在HVPE反应器中进行衬底表面的这种氮化。在美国专利No.6528394中公开了使用氨(NH3)-氯化氢(HCl)气体混合物的氮化技术，在本发明中引入并作为参考。
在950到1100℃的生长温度范围内和以30到300μm/hr的生长速度通过HVPE在r-面衬底上生长的a-面氮化物膜允许在氮化物膜表面中出现<0001>取向的脊，以便彼此聚合，导致所希望的无空隙a-面氮化物厚膜的形成。
此外，这种a-面氮化物膜生长由于如图3中所示的内部应力的大的各向异性，导致在下面的衬底内部形成微空隙。在衬底内部形成的微空隙不互相连接但是会产生作用以减少在氮化物膜中产生的内部应力，由此对衬底或在其上形成的氮化物膜的形状不产生负面影响。
这样，在本发明方法中，可以生长无任何空隙、翘曲和裂纹的a-面氮化物厚膜，其具有130μm或更厚的厚度、优选150μm或更厚、更优选为300μm或更厚以及25mm的直径、优选50.8mm(2英寸)的直径。具体地，可以生长厚度不受限制的氮化物膜。
然后，可以从衬底分离生长的a-面氮化物膜，并且可以通过常规方法来抛光分离的氮化物膜的表面，以获得改善的具有光滑表面的a-面氮化物晶圆。
如上所述，本发明第一次提供一种无空隙、翘曲或裂纹的高质量的非极性单晶a-面氮化物半导体晶圆，该晶圆可以用作制造发光二极管(LED)的独立的基板。
以下实施例仅仅用于说明的目的，且不想限制本发明的范围。
实例1
在HVPE反应器中，放置50.8mm直径的单晶r-面蓝宝石衬底，并且依次用气态的氨、氨和氯化氢的气体混合物和气态的氨在950到1100℃下进行氮化。
在这样获得的氮化衬底上，通过使气态的氯化镓和气态的氨在1000℃下与其接触，允许氮化镓单晶膜以75μm/hr的速度进行生长。按照1∶6的气态氯化氢∶气态氨的体积比通过两个隔离的入口引入由镓与氯化氢反应所产生的氯化镓气体和气态的氨，。在环境压力之下，反应器腔保持在600到900℃的温度范围内。进行氮化镓单晶膜的生长400分钟，以便在衬底上形成500μm厚的氮化镓半导体膜。
图4和5分别示出这样形成的a-面GaN厚膜的照片和X射线衍射(XRD)图形。图7A和7B分别示出其表面的扫描电子显微镜(SEM)照片和XRD振动曲线。图7B的XRD振动曲线表明已获得了一种具有871弧度秒的FWHM(半最高幅度的全宽度)值的a-面氮化物膜。
然后，采用355nm的Q切换Nd:YAG受激准分子激光器，从衬底分离生长的a-面氮化物膜。采用晶圆研磨和抛光机器，抛光分离的氮化物膜，从而获得400μm厚的氮化镓独立的基板。
图6示出所获得的a-面GaN基板的照片，已经证实其是没有表面缺陷的光滑基板。
实例2
除了气态氯化氢和气态氨的体积比在1∶2～5的范围内之外，重复实例1的步骤，在蓝宝石衬底上形成500μm厚的氮化镓半导体膜。
图8A和8B分别示出这样形成的a-面GaN厚膜表面的SEM照片和XRD振动曲线。图8B的XRD振动曲线显示a-面氮化物膜具有342弧度秒的FWHM值，在迄今报道的FWHM值中为最小值，这表示显著地提高了膜的结晶性。
如上所述，根据本发明的方法，可以快速并有效地制备无空隙、翘曲或裂纹的高质量的非极性单晶a-面氮化物半导体晶圆，并且它可以有利地用作LED制造中的衬底。
虽然已经关于上述具体的实施例对本发明进行了说明，但是应当认识到，本领域技术人员可以对本发明进行各种修改和变化，并且这些修改和变化同样落入附加权利要求所限定的本发明的范围之内。

Claims (18)

1、一种单晶a-面({11-20}面)氮化物半导体晶圆，具有130μm或更大的厚度。
2、根据权利要求1所述的a-面氮化物半导体晶圆，该a-面氮化物半导体晶圆具有150μm或更大的厚度。
3、根据权利要求1所述的a-面氮化物半导体晶圆，该a-面氮化物半导体晶圆具有300μm或更大的厚度。
4、根据权利要求1所述的a-面氮化物半导体晶圆，在单晶r-面({1-102}面)蓝宝石衬底上生长该a-面氮化物半导体晶圆。
5、根据权利要求1所述的a-面氮化物半导体晶圆，通过氢化物气相外延(HVPE)生长该a-面氮化物半导体晶圆。
6、根据权利要求1所述的a-面氮化物半导体晶圆，该a-面氮化物半导体晶圆具有25mm或更大的直径。
7、根据权利要求1所述的a-面氮化物半导体晶圆，该a-面氮化物半导体晶圆具有50.8mm或更大的直径。
8、根据权利要求4所述的a-面氮化物半导体晶圆，在生长之后，从所述衬底分离该a-面氮化物半导体晶圆，然后进行抛光。
9、根据权利要求1所述的a-面氮化物半导体晶圆，该a-面氮化物半导体晶圆在X射线衍射(XRD)振动曲线中具有1000arcsec或更小的FWHM(半最高幅度的全宽度)值。
10、根据权利要求1所述的a-面氮化物半导体晶圆，该a-面氮化物半导体晶圆在X射线衍射(XRD)振动曲线中具有500arcsec或更小的FWHM(半最高幅度的全宽度)值。
11、根据权利要求1所述的a-面氮化物半导体晶圆，该a-面氮化物半导体晶圆用作发光二极管制造中的独立的基板。
12、根据权利要求1所述的a-面氮化物半导体晶圆，该a-面氮化物半导体晶圆由选自Ga、Al和In组成的组中的至少一种III族元素的氮化物构成。
13、一种用于制备根据权利要求1所述的a-面氮化物晶圆的方法，包括：通过氢化物气相外延(HVPE)，以30到300μm/hr的速度在加热至950到1100℃的温度范围的单晶r-面蓝宝石衬底上生长所述a-面氮化物膜，从所述衬底分离所述已生长的a-面氮化物膜，并且抛光其表面。
14、根据权利要求13所述的方法，其中通过在反应器腔中使III族元素的氯化物蒸汽和气态氨(NH3)与所述衬底的表面接触，来进行该a-面氮化物膜的生长，通过该III族元素和气态氯化氢之间的反应来产生该III族元素的氯化物蒸汽。
15、根据权利要求14所述的方法，其中该气态氯化氢和气态氨的体积比处于1∶2～20的范围内。
16、根据权利要求14所述的方法，其中该气态氯化氢和气态氨的体积比处于1∶2～5的范围内。
17、根据权利要求13所述的方法，其中通过用氨(NH3)和氯化氢(HCl)的气体混合物进行处理来氮化用于生长的该r-面蓝宝石衬底的表面。
18、根据权利要求13所述的方法，其中连续生长该a-面氮化物膜，直到获得所希望的厚度。
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CN100377306C (zh) 2008-03-26
DE602005024742D1 (de) 2010-12-30
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KR20060045834A (ko) 2006-05-17
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EP1593760A1 (en) 2005-11-09
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