CN103928501B - 基于m面GaN上的极性InN纳米线材料及其制作方法 - Google Patents

基于m面GaN上的极性InN纳米线材料及其制作方法 Download PDF

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CN103928501B
CN103928501B CN201410165353.7A CN201410165353A CN103928501B CN 103928501 B CN103928501 B CN 103928501B CN 201410165353 A CN201410165353 A CN 201410165353A CN 103928501 B CN103928501 B CN 103928501B
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许晟瑞
姜腾
郝跃
杨林安
张进成
林志宇
樊永祥
张春福
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Abstract

本发明公开了一种基于m面GaN上的极性InN纳米线材料及其制作方法，主要解决常规极性InN纳米线生长中工艺成本高、效率低、方向一致性差的问题。其生长步骤是：(1)在m面GaN衬底上蒸发一层1‑15nm金属Ti；(2)将有金属Ti的m面GaN衬底置于MOCVD反应室中，并向反应室内通入氢气与氨气，使m面GaN衬底上的一部分金属Ti氮化形成TiN，并残余一部分未被氮化的金属Ti；(3)向MOCVD反应室中同时通入铟源和氨气，利用未被氮化的金属Ti作为催化剂在TiN层上生长平行于衬底、方向一致的极性InN纳米线。本发明具有成本低，生长速率快，方向一致性好的优点，可用于制作高性能极性InN纳米器件。

Description

基于m面GaN上的极性InN纳米线材料及其制作方法
技术领域
本发明属于微电子技术领域，涉及半导体材料的生长方法，特别是一种m面GaN上的极性InN纳米线的金属有机物化学气相外延生长方法，可用于制作InN纳米结构半导体器件。
技术背景
InN作为III族氮化物半导体的一种，自20世纪八十年代以来，由于其优异的性能受到了研究者极大的关注。作为一种直接带隙半导体，禁带宽度为0.7eV的InN在长波长半导体光电器件、太阳能电池等方面有着良好的应用前景。在Ⅲ族氮化物中，由于InN高的迁移率、高饱和速率、大的电子漂移速率以及具有最小的有效电子质量等性质，使得InN一维纳米结构在高频器件、激光二极管等方面有着独特的优势，因此，InN纳米线的制备成为人们研究的热点。
2005年Shudong Luo等人采用化学气相沉积CVD方法制备了InN纳米线，参见LuoS,Zhou W,Zhang Z,et al.Synthesis of long indium nitride nanowires withuniform diameters in large quantities[J].Small,2005,1(10):1004-1009.这种方法虽然获得了直径一致的InN纳米线，但由于其生长时间长，生长速率低，方向一致性差，限制了InN纳米线的器件应用。
2006年T Stoica等人采用分子束外延MBE方法成功制备了InN纳米线，参见StoicaT,Meijers R,Calarco R,et al.MBE growth optimization of InN nanowires[J].Journal of crystal growth,2006,290(1):241-247.虽然MBE法制备的InN纳米线方向一致性好，但由于纳米线长度较短，且MBE设备成本高，因此该方法不适合工业大规模生产。
发明内容
本发明的目的在于针对上述已有技术的不足，提供一种基于m面GaN衬底的极性InN纳米线材料及其制作方法，以降低制备成本，提高生长效率，为制作高性能极性InN纳米器件提供材料。
实现本发明目的技术关键是：在非极性m面GaN上采用Ti金属催化的方法，通过调节生长的压力、流量、温度，实现高速，高质量，平行于衬底且方向一致性很好的极性InN纳米线，其技术方案如下：
一.本发明基于m面GaN上的极性InN纳米线材料，自下而上包括m面GaN衬底层和极性InN纳米线层，该极性InN纳米线层中含有若干条平行于衬底、方向一致且长度不等的纳米线，其特征在于在m面GaN衬底层的上面设有1-15nm厚的TiN层，极性InN纳米线层位于该TiN层的上面。
所述m面GaN衬底层的厚度为1-1000μm。
所述极性InN纳米线层中的每条纳米线的长度在1-100μm范围内随机产生。
二.本发明基于m面GaN极性纳米线材料的制作方法，包括如下步骤：
(1)将厚度为1-1000μm的m面GaN衬底放入电子束蒸发台E-Beam中，在真空度为1.8×10-3Pa的条件下，以0.2nm/s的速度蒸发一层1-15nm的Ti金属薄膜；
(2)将有Ti金属的m面GaN衬底置于金属有机物化学气相淀积MOCVD反应室中，并向反应室内通入流量均为1000sccm-10000sccm的氢气与氨气，对衬底基片进行氮化处理，即将m面GaN衬底上的一部分金属Ti氮化形成TiN，并残余一部分未被氮化的金属Ti；
(3)向MOCVD反应室中同时通入流量为5-100μmol/min的铟源和1000-10000sccm的氨气，利用未被氮化的金属Ti作为催化剂在TiN层之上生长若干条平行于衬底且长度不等的极性InN纳米线，其生长的工艺条件是：温度为400-900℃，时间为5-60min，反应室内压力为20-760Torr。
(1)在厚度为1-1000μm的m面GaN衬底上蒸发一层1-15nm的Ti金属；
(2)将有Ti金属的m面GaN衬底置于金属有机物化学气相淀积MOCVD反应室中，并向反应室内通入流量均为1000sccm-10000sccm的氢气与氨气，在温度为600-1200℃，时间为5-20min，反应室压力为20-760Torr的工艺条件下，使m面GaN衬底上的一部分金属Ti氮化形成1-15nm厚的TiN，并残余一部分未被氮化的金属Ti；
(3)向MOCVD反应室中同时通入流量为5-100μmol/min的铟源和1000-10000sccm的氨气，利用未被氮化的金属Ti作为催化剂在TiN层之上生长若干条平行于衬底且长度为1-100μm不等的极性InN纳米线，每条纳米线的长度根据残留的金属Ti液滴大小，以及生长的工艺条件随机产生。
所述的利用未被氮化的金属Ti作为催化剂在TiN层之上生长若干条平行于衬底且长度为1-100μm不等的极性InN纳米线，其工艺条件是：
温度：400-900℃；
时间：5-60min；
反应室内压力：20-760Torr。
本发明具有如下优点：
1.工艺成本低，生长速率快，且方向一致性好。
2.采用非极性m面GaN材料作为衬底，由于在m面GaN材料中极性轴c轴在面内，使得生长过程中，铟源和氨气分子在表面沿极性轴方向迁移时得以充分反应，有利于获得较长的高质量极性InN纳米线结构。
3.通过氮化形成TiN层，并利用残余的未被氮化的Ti金属作为催化剂生长纳米线，大大提高了生长速率。
本发明的技术方案和效果可通过以下附图和实施例进一步说明。
附图说明
图1为本发明基于m面GaN的极性InN纳米线材料结构示意图；
图2是本发明制作基于m面GaN的极性InN纳米线材料的流程图。
具体实施方式
参照图1，本发明的材料结构自下而上依次为m面GaN衬底层，TiN层和极性InN纳米线层。其中m面GaN衬底层的厚度为1-1000μm，TiN层的厚度为1-15nm，极性InN纳米线层中的若干条纳米线平行于衬底、方向一致，每条纳米线的长度在1-100μm范围内不等。
本发明制作图1所述材料的方法给出三种实施例：
实施例1，制备TiN层厚度为8nm的极性InN纳米线材料。
参照图2，本实例的实现步骤如下：
步骤1，将厚度为5μm的m面GaN衬底放入电子束蒸发台E-Beam中，在真空度为1.8×10-3Pa的条件下，以0.2nm/s的速度蒸发一层10nm的Ti金属薄膜。
步骤2，制备TiN层。
将有Ti金属的m面GaN衬底置于金属有机物化学气相淀积MOCVD反应室中，抽真空后设置反应室内压力为40Torr，加热温度为900℃，再向反应室内通入流量为3000sccm的氢气和流量为3000sccm的氨气，持续8min，使大部分金属Ti与氨气反应，在m面GaN衬底上形成厚度为10nm的TiN层，并有少部分未与氨气发生反应的残留金属Ti，随机分布在TiN层表面。
步骤3，生长极性InN纳米线。
对反应室继续加热，使已形成了TiN层的m面GaN衬底温度升高到1200℃，再向反应室内同时通入流量为40μmol/min的铟源、流量为3000sccm的氢气和流量为3000sccm的氨气，保持反应室压力不变，持续15min，用分布在TiN层的残留金属Ti作为催化剂，在TiN层上，从这些残留金属Ti的位置起源，生长出若干条平行于衬底、方向一致且长度不等的极性InN纳米线，每条纳米线的长度根据残留的金属Ti液滴大小，以及生长的工艺条件在1-100μm范围内随机产生。
步骤4，待反应室温度降至常温后，将通过上述步骤生长的极性InN纳米线材料从MOCVD反应室中取出。
实施例2，制作TiN层厚度为1nm的极性InN纳米线材料。
参照图2，本实例的实现步骤如下：
步骤A，将厚度为1μm的m面GaN衬底放入电子束蒸发台E-Beam中，在真空度为1.8×10-3Pa的条件下，以0.2nm/s的速度蒸发一层1nm的Ti金属薄膜。
步骤B，制备TiN层。
将有Ti金属的m面GaN衬底置于金属有机物化学气相淀积MOCVD反应室中，抽真空后设置反应室压力和加热温度，再向反应室内同时通入氢气和氨气，持续一段时间，使大部分金属Ti与氨气反应，在m面GaN衬底上形成厚度为1nm的TiN层，并有少部分未与氨气发生反应的金属Ti，随机分布在TiN层表面，其中氢气和氨气的流量均为1000sccm，反应室内压力为20Torr，加热温度为600℃，持续时间为5min。
步骤C，生长极性InN纳米线。
对反应室继续加热，使已形成了TiN层的m面GaN衬底温度升高到800℃，保持反应室压力不变，向反应室内同时通入铟源，氢气和氨气，持续一段时间，用分布在TiN层的残留金属Ti作为催化剂，在TiN层上，从金属Ti位置起源，生长出若干条平行于衬底、方向一致的极性InN纳米线，每条纳米线的长度根据残留的金属Ti液滴大小，以及生长的工艺条件在1-100μm范围内随机产生，其中铟源流量为5μmol/min，氢气和氨气的流量均为1000sccm，持续时间为5min。
步骤D，待反应室温度降至常温后，将通过上述步骤生长的极性InN纳米线材料从MOCVD反应室中取出。
实施例3，制作TiN层厚度为15nm的极性InN纳米线材料。
参照图2，本实例的实现步骤如下：
第一步，蒸发金属Ti薄膜。
将厚度为1000μm的m面GaN衬底放入电子束蒸发台E-Beam中，在真空度为1.8×10- 3Pa的条件下，以0.2nm/s的速度蒸发一层15nm的Ti金属薄膜。
第二步，制备TiN层。
在金属有机物化学气相淀积MOCVD反应室中放置有Ti金属的m面GaN衬底，抽真空后加热反应室，使温度达到1200℃，在反应室压力为760Torr的条件下，同时向反应室内通入流量均为10000sccm氢气和氨气，持续60min，使大部分金属Ti与氨气反应，在m面GaN衬底上形成厚度为15nm的TiN层，其有少部分未与氨气发生反应的金属Ti，随机分布在TiN层表面。
第三步，生长极性InN纳米线。
在反应室内压力为760Torr的条件下，将已形成了TiN层的m面GaN衬底温度升高到1500℃，向反应室内同时通入流量均为10000sccm的氢气和氨气以及100μmol/min的铟源，持续时间为60min，用分布在TiN层的残留金属Ti作为催化剂，在TiN层上，从这些金属Ti位置起源，生长出若干条平行于衬底、方向一致的极性InN纳米线，每条纳米线的长度根据残留的金属Ti液滴大小，以及生长的工艺条件在1-100μm范围内随机产生。
第四步，待反应室温度降至常温后，将通过上述步骤生长的极性InN纳米线材料从MOCVD反应室中取出。

Claims (2)

1.一种基于m面GaN的极性InN纳米线材料制作方法，包括如下步骤：
(1)在厚度为1-1000μm的m面GaN衬底上蒸发一层1-15nm的Ti金属；
(2)将有Ti金属的m面GaN衬底置于金属有机物化学气相淀积MOCVD反应室中，并向反应室内通入流量均为1000sccm-10000sccm的氢气与氨气，在温度为600-1200℃，时间为5-20min，反应室压力为20-760Torr的工艺条件下，使m面GaN衬底上的一部分金属Ti氮化形成1-15nm厚的TiN，并在TiN表面残余一部分未被氮化的金属Ti；
(3)向MOCVD反应室中同时通入流量为5-100μmol/min的铟源和1000-10000sccm的氨气，利用未被氮化的金属Ti作为催化剂在TiN层之上生长若干条平行于衬底且长度为1-100μm不等的极性InN纳米线，每条纳米线的长度根据残留的金属Ti液滴大小，以及生长的工艺条件随机产生。
2.根据权利要求1所述的方法，其中步骤(3)所述的利用未被氮化的金属Ti作为催化剂在TiN层之上生长若干条平行于衬底且长度为1-100μm不等的极性InN纳米线，其工艺条件是：
温度：400-900℃；
时间：5-60min；
反应室内压力：20-760Torr。
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