CN110364420A - 一种插入InGaN/GaN超晶格结构改善非极性GaN材料质量的外延生长方法 - Google Patents

一种插入InGaN/GaN超晶格结构改善非极性GaN材料质量的外延生长方法 Download PDF

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CN110364420A
CN110364420A CN201910639441.9A CN201910639441A CN110364420A CN 110364420 A CN110364420 A CN 110364420A CN 201910639441 A CN201910639441 A CN 201910639441A CN 110364420 A CN110364420 A CN 110364420A
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韩军
赵佳豪
邢艳辉
崔博垚
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Abstract

本发明提供一种插入InGaN/GaN超晶格结构改善非极性GaN材料外延质量的方法，是一种减小非极性GaN材料位错密度，改善外延片表面形貌，从而提高材料质量的外延生长方法。利用金属有机物化学气相沉积(MOCVD)技术，外延结构从下向上依次为，r面蓝宝石衬底，低温GaN成核层；高压、高V/III比(V族与III族源摩尔流量比)生长条件生长的高温三维GaN层；第一次低压、低V/III比生长条件生长的高温二维GaN层；InGaN/GaN超晶格结构插入层；第二次低压、低V/III比生长条件生长的高温二维GaN层。本发明的特点是在二维GaN层中插入InGaN/GaN超晶格结构插入层，其能够缓解应力，并且阻挡部分蓝宝石衬底与外延生长的GaN材料失配产生的穿透位错传递。本发明能够减小非极性GaN材料位错密度，改善表明形貌，提高外延片的质量。

Description

一种插入InGaN/GaN超晶格结构改善非极性GaN材料质量的外 延生长方法
技术领域：
本发明属于GaN材料外延技术领域，涉及一种提高非极性GaN材料质量，减少位错的技术。
背景技术：
氮化镓(GaN)是直接带隙材料，具有禁带宽，化学性质稳定，耐高温的特点，广泛应用于发光器件、光电探测器、太阳能电池等器件。目前商业化生产的GaN器件，都是在c面蓝宝石衬底上制备的GaN器件，它们都是沿极性轴c轴生长的，材料存在极化效应，其器件有源区内会出现很强的极化电场，致使电子空穴对分离，出现量子限制斯塔克效应，导致发光效率的降低。为了避免发生极化效应，可以生长非极性GaN材料和器件，非极性GaN材料是指生长方向垂直于极性轴[0001]方向,如沿[1120]方向生长，非极性GaN薄膜可以消除极化电场，有利于提高器件的量子效率。但是由于沿[1120]方向生长的a面非极性GaN材料，位于生长面内的c轴[0001]和m轴[1100]方向，晶格常数不同，会带来不同的失配，沿c轴的失配是1.2％，而沿m轴的失配是16％，所以非极性外延材料存在各向异性，位错密度高的问题，结果造成外延非极性GaN材料质量距离实际应用有较大差距。目前非极性GaN薄膜存在两个主要问题，粗糙的表面形貌，较高的位错层错密度。这是限制非极性GaN基器件性能参数的主要因素，使非极性GaN基器件的优势不能明显的表现出来。
许多在位减少缺陷技术被应用于非极性GaN材料的生长，如衬底氮化、各种生长条件的优化，两步生长法，SiN插入层技术和图形衬底技术，其中两步生长法(控制生长条件，第一步生长三维GaN层减小位错，然后第二步转换为两维GaN生长改善表面形貌)是一种简单有效的减少位错的方法，但是也存在问题，如要想有效减少位错，三维GaN层要长的尽可能厚，但是过厚的三维GaN层，会使表面非常粗糙，后面的两维GaN层即使很厚，无法完全改善表面形貌，给后续的器件生长带来负面影响。
所以，有必要提供一种基于蓝宝石衬底获得位错密度小、表面形貌好、能够改善非极性GaN薄膜质量的方法，用以解决上述问题。本发明采用插入InGaN/GaN超晶格结构改善非极性GaN材料质量的外延生长方法，可以改进目前两步生长法存在的问题，进一步提高材料质量。
发明内容：
本发明的目的在于改善现有技术的不足，通过金属有机物化学气相沉积(MOCVD)方法，提高在蓝宝石衬底上生长的非极性a面GaN薄膜材料质量，减少位错密度，改善表面形貌。其生长步骤如下：
步骤一：将r面蓝宝石衬底放入MOCVD反应室中的衬底托上，在温度1000℃—1100℃，烘烤3-10分钟
步骤二：在温度1000℃—1100℃，氮气和氨气体积比例为2比1的混合气氛中，氮化2-10分钟。
步骤三：降低温度到500℃—600℃，压力500-600mbar，生长一层厚度20-40nm的低温成核层。
步骤四：升温到1000℃—1100℃，压力300-600mbar，V/III比1000-3000，生长高压、高V/III比三维GaN层，厚度1μm-2μm。
步骤五：在温度1000℃—1100℃，压力,50-200mbar，V/III比50-300，第一次生长低压、低V/III比二维GaN层，厚度1μm-2μm。
步骤六：降低温度到700℃—800℃，生长InGaN/GaN超晶格结构，其中InGaN层的In组分为5％-20％。厚度5-20nm，GaN层厚度5-10nm，先生长一层上述的GaN层，然后生长上述组分和厚度的InGaN层，交替生长上述GaN层和InGaN层共3-20周期，最后生长一层5-20nm的GaN层；
步骤七：升温到1000℃—1100℃，压力50-200mbar，V/III比50-300，第二次生长低压、低V/III比二维GaN层，厚度2μm-5μm。
其特征是生长方法是金属有机物化学气相沉积方法，三甲基镓或三乙基镓为镓源，三甲基铟为铟源，氨气为氮源，载气为氢气及氮气。
本发明的机理特点在于：利用MOCVD生长技术，在r面蓝宝石衬底上，通过两步生长法(先生长三维GaN层，再在此基础上生长二维GaN层)并引入InGaN/GaN超晶格插入层，将InGaN/GaN超晶格层插入到二维GaN层中间。目前常用的方法是两步生长法，在高压，高V/III比条件下生长三维非极性GaN薄膜，但是表面形貌较为粗糙，在此基础上低压，低V/III比条件下生长二维非极性GaN薄膜，可以改善表面形貌，减少位错密度。但是通过两步生长法生长的非极性GaN薄膜位错密度仍然较高，不利于半导体器件的工作。于是本发明，在两步生长法的基础上，在两维GaN层中间，引入InGaN/GaN超晶格结构插入层，InGaN/GaN超晶格插入层具有缓解因晶格常数不同而产生的应力，改变位错传递方向从而截断部分位错的能力,阻挡了大部分蓝宝石衬底与GaN外延层失配产生的穿透位错的传递。因此生长的非极性GaN薄膜位错密度较低，表面形貌较好。可以在原来两步生长法基础上，进一步减少位错，改善非极性GaN材料的质量。
附图说明
图1是本发明将InGaN/GaN超晶格结构插入层插入至二维GaN层之间的生长结构示意图
图2是未插入InGaN层样品的(1120)面沿c轴x射线衍射ω扫描图
图3是插入InGaN/GaN超晶格结构插入层的样品(具体实施案例1)的(1120)面沿c轴x射线衍射ω扫描图
图4是未插入InGaN层样品的原子力显微镜表面形貌图
图5是插入InGaN/GaN超晶格结构插入层的样品(具体实施案例1)的原子力显微镜表面形貌图
具体实施方式
下面结合具体实施案例1，并附图，对本发明作进一步地说明：
本案例是通过金属有机物化学气相沉积(MOCVD)方法在r面蓝宝石衬底上插入InGaN/GaN超晶格结构插入层改善非极性a面GaN薄膜的质量，减少位错密度，改善表面形貌。如图1所示，将InGaN/GaN超晶格结构插入层插入至二维GaN层之间，具体实验步骤如下：
其生长步骤如下：
步骤一：将r面蓝宝石衬底放入MOCVD反应室中的衬底托上，在温度1050℃，烘烤3分钟
步骤二：在温度1050℃，氮气和氨气体积比例为2比1的混合气氛中，氮化10分钟。
步骤三：降低温度到550℃，压力500mbar，生长一层厚度40nm的低温成核GaN层。
步骤四：升温到1050℃，压力500mbar，V/III比3000，生长高压、高V/III比三维GaN层，厚度2μm。
步骤五：在温度1050℃，压力，50mbar，V/III比100，第一次生长低压、低V/III比二维GaN层，厚度2μm。
步骤六：降低温度到750℃，生长InGaN/GaN超晶格结构插入层，其中InGaN层的In组分10％。厚度10nm，GaN层厚度5nm，先生长一层上述GaN层，然后生长一层InGaN层，交替生长GaN层和InGaN层共20周期，最后生长一层5nm的GaN层；
步骤七：升温到1050℃，压力50mbar，V/III比100，第二次生长低压、低V/III比二维GaN层，厚度5μm。
生长方法是金属有机物化学气相沉积方法，三甲基镓为镓源，三甲基铟为铟源，氨气为氮源，载气为氢气及氮气。
测试结果，图2是未插入InGaN层样品的(1120)面沿c轴x射线衍射ω扫描图，半宽为1148arcsec；图3是插入InGaN/GaN超晶格结构插入层的样品(具体实施案例1)的(1120)面沿c轴x射线衍射ω扫描图，半宽为1012arcsec，比未插入InGaN层样品半宽减少了136arcsec；说明插入InGaN/GaN超晶格结构改善了材料质量。
图4是未插入InGaN层样品的原子力显微镜表面形貌图，表面均方根粗糙度为1.01nm；图5是插入InGaN/GaN超晶格结构插入层的样品(具体实施案例1)的原子力显微镜表面形貌图，表面均方根粗糙度为0.88nm；插入InGaN/GaN超晶格结构插入层后的具体实施案例1样品，减小了粗糙度，表面更加平坦。
实施案例1制作的非极性GaN薄膜位错密度较低，表面形貌较好。提高了非极性GaN材料质量，改善了现有技术的不足。
最后应说明的是：以上事实案例为本发明的通常实施方案，而非对其限制；任何对前述各实施案例的技术方案进行的简单变化或修饰，或对其中部分或者全部技术进行等同替换，都应包括在本发明的保护范围内。

Claims (1)

1.一种插入InGaN/GaN超晶格结构改善非极性GaN材料外延质量的方法，其特征在于，外延片结构从下向上依次为；r面蓝宝石衬底生长GaN成核层后，生长高压、高V/III比生长条件生长的高温三维GaN层；第一次低压、低V/III比生长条件生长的高温二维GaN层；InGaN/GaN超晶格结构插入层；第二次低压、低V/III比生长条件生长的高温二维GaN层；
所述的高压、高V/III比生长条件生长的高温三维GaN层，生长温度1000℃—1100℃，压力300-600mbar，V/III比即V族与III族源摩尔流量比为1000-3000，厚度1μm-2μm；
所述的第一次低压、低V/III比生长条件生长的高温二维GaN层，生长温度1000℃—1100℃，压力,50-200mbar，V/III比50-300，厚度1μm-2μm；
所述的InGaN/GaN超晶格结构插入层，生长温度700℃—800℃，其中InGaN层中的In组分的摩尔百分比在5％-20％，先生长一层厚度5-20nm GaN层，然后生长上述In组分的厚度5-20nm的InGaN层，交替生长上述GaN层和InGaN层3-20周期，最后生长一层5-20nm的GaN层；
所述的第二次低压、低V/III比生长条件生长的高温二维GaN层，生长温度1000℃—1100℃，压力,50-200mbar，V/III比50-300，厚度2μm-5μm。
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